P. 1
PiroGl

PiroGl

|Views: 2|Likes:
Published by Saroj Manandhar
Preservatives put in the topical gels are harmful and may pose threat to woman breast health. Cases of Methylparaben and propylparaben getting accumulated in the woman breast have been reported with possible risk of cancer
Preservatives put in the topical gels are harmful and may pose threat to woman breast health. Cases of Methylparaben and propylparaben getting accumulated in the woman breast have been reported with possible risk of cancer

More info:

Categories:Types, Reviews
Published by: Saroj Manandhar on Jun 10, 2013
Copyright:Attribution Non-commercial

Availability:

Read on Scribd mobile: iPhone, iPad and Android.
download as DOC, PDF, TXT or read online from Scribd
See more
See less

06/15/2013

pdf

text

original

PIROXICAM GEL

No 1. 2. 3. 4 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. Description Drug Authority Application form Name and Address of Applicant *& Manufacturer Name of the Product Free Sale certificate Certificate Certificate of the composition of the product giving in detail the chemistry of the active ingredient / ingredient of the product. Detailed specification and standards laid down by the manufacturer for each product together with its method of analysis in details. A certificate of sterility and absence of pyrogen wherever it is applicable Six samples of the product applied for registration in their original pack. Certificate of Analysis Reference Sample Bioavailability studies I Safety and Tolerance studies & Test Detailed Reports covering a) Pharmacological b) Toxicological c) Clinical aspects Storage Date Authenticated price list Name of the competitive drugs manufactured by other firms Other countries where the product is Registered Date of introduction of the product to the market in the country of origin. Section No

I II ill IV V VI VII VIII IX X XI XII XIII XIV XV XIV

COMPOSITION OF THE PRODUCT

PRODUCT : ROXICAM GEL Batch No. :01

Batch Size : 300.0 kgs

NO 1 2 3 4 5 6 7 8 9

INGREDIENTS Piroxicam Carbomer 934 Glycerin Propylene glycol Potassium Hydroxide Disodium Edetate Methyl Paraben Propyi Paraben D.M.Water Q.S. to

SPEC. IP USP IP IP IP IP IP IP IP

LABEL CLAIM W/W 0.50 % 0.90 % 10.00 % 20.00 % 0.80 % 0.01 % 0.16% 0.04 %

OVER AGES 5.0 % — — — — — — — —

QTY IN KGS 1.575 2.700 30.000 60.000 2.400 0.030 0.480 0.120 300.000

CHEMICAL NAME & STRUCTURAL FORMULA OF EACH ACTIVE INGREDIENT

DRUG NAME SYNONYM MOLECULAR FORMULA CHEMICAL NAME

:

Piroxicam

: :

C15Hi3N304S 4-hydroxy-2-methyl-N-(2-pyridyl)-2H-1,2benzothiazine -3-carboxamide-l,l-dioxide I.P - 1996 ; Page No. 600

SPECIFICATION OR REFERENCE TEXT

:

INACTIVE INGREDIENTS
PRODUCT: ROXICAM GEL Batch No. :01

Batch Size : 300.0 kgs

NO 1 2 3 4 5 6 7 8

INGREDIENTS Carbomer 934 Glycerin Propylene glycol Potassium Hydroxide Disodium Edetate Methyl Paraben Propyi Paraben D.M.Water Q.S.to

SPE. USP IP IP IP IP IP IP IP

LABEL CLAIM 0.90 % 10.00% 20.00% 0.80% 0.01% 0.16% 0.04%

OVER AGES — — — — — — — —

QTY IN KGS 2.700 30.000 60.000 2.400 0.030 0.480 0.120 300.00

REASON FOR INCLU. Suspending & gelling agent Humectant Humectant & solvent PH adjuster Chelating/com plexing agent. Antimicrobial preservative Antimicrobial Preservative Solvent

RAW MATERIAL SPECIFICATION AND ANALYTICAL CONTROL PROCEDURE .

CATEGORY: Analgesic.0 percent ofC15H13N3O4S. DOSE : 10 to 20 mg daily.2. very slightly soluble in water. calculated with reference to the anhydrous substance. STANDARDS: Piroxicam contains not less than 97. DESCRIPTION : Off-white to light tan or light yellow powder.Wt.1996 PAGE : 01 OF 03 C15H13N304S Mol. STORAGE: Store in tightly-closed.dioxide.1. 331. antipyretic. SOLUBILITY: Slightly soluble in ethanol (95%) and in aqueous alkaline solutions.RAW MATERIAL : PIROXICAM PROTOCOL : IP . .35 Piroxicam is 4-hydroxy-2-metfayl-N-(2-pyridyl)-2H-l. in dilute acids and in most organic solvents.0 per cent and not more than 103.benzothiazine -3-carboxamide1. antiinflammatory. light resistant containers . odourless.

02 OF 03 The infrared absorption spectrum. After removal of the plate allow it to dry in air and examine under ultra-violet light (254 nm).22. C. . absorbance at about 334 nm.1996 IDENTIFICATION : A. is concordant with the reference spectrum of piroxicam or with the spectrum obtained from piroxicam RS. Appendix 5. HEAVY METALS: Not more than 50 ppm.6. The principal spot in the chromatogram obtained with solution (1) corresponds to that in the chromatogram obtained with solution (2). about 0.5.01 M methanolic hydrochloric acid exhibits two maxima. Appendix 5. Appendix 3. PAGE .1 % w/v of piroxicam RS .87. using silica gel GF254 as the coating substances and a mixture of 95 volumes of toluene and 5 volumes of acetic acid as the mobile phase but allowing the solvent front to ascend 15 cm above the line of application. SULPHATED ASH : Not more than 0. B.RAW MATERIAL : PIROXICAM PROTOCOL : IP . Carry out the method for thin layer chromatography. at about 242 nm and 334 nm and a minimum at about 270 nm.4 g by Method B. determined on 0.1 % w/v of the substance being examined.4.3 %. The light absorption in the range 230 to 360 nm of a 0.. Allow it to dry and develop again. Appendix 3. Apply separately to the plate 20 jul of each of the two solutions in a mixture of equal volumes of chloroform and methanol containing (1) 0. (2) 0.001% w/v Solution in 0. Appendix 4.12.

RAW MATERIAL : PIROXICAM PROTOCOL : IP - 1996

PAGE : 03 OF 03

WATER: Not more than 0.5 %w/w, determined on 2.0 g, Appendix 3.24. ASSAY: Carry out the method for high performance liquid chromatography, Appendix 4.3, using die following solutions in 0.1 M methanolic hydrochloric acid containing (1) 0.005% w/v of the substance being examined and (2) 0.005 % w/v of piroxicam RS. The Chromatographic procedures may be carried out using (a) a stainless steel column packed with stationary phase LCI, (b) a degassed mixture of 45 volumes of methanol and 55 volumes of a buffer solution prepared by diluting a mixture of 7.72 g of anhydrous citric acid in 400 ml of water and 5.35 g of sodium phosphate in 100 ml of water to 1000 ml with water as the mobile phase with a flow rate of 1.2 ml per minute and (c) a detection wavelength of about 254 run. The column efficiency determined using solution (2) is not less than 500 theoretical plates, the tailing factor is not more than 1.5. The test is not valid unless the relative standard deviation for replicate injections is not more than 2.0 %. Calculate me content of C15H13N3O4S in piroxicam RS.

TEST CERTIFICATE (THE DRUGS AND COSMETICS ACT 1940 AND THE RULES THEREUNDER FORM 39 ) RAW MATERIAL : PIROXICAM IP Party : Universal Impex A.R.NO. : UIR 257/98-99 G.R.N.no. : UI/RM/250/989 Pub. Lab. T.R.NO. : R07556 Batch No. : PX-036/98 Mfg. Date : Dec' 1998 Batch Size : 1x5 kg = 5 kg Exp. Date : Nov'2003 Manufacturer: Ramdev Chem Dt of Receipt : 24/01/99 Supplier : ReamdevChem Dtof Completion : 30/01/99 Ch.No./Dt : 243/24-01-99 Qty sampled : 2x5g RESULTS OF ANALYSIS & PROTOCOLS OF TEST APPLIED AS PER IP-96 Protocols Description Solubility Identification A,B,C Heavy metals. Sulphated ash Water Assay as C15H13N3O4S Results Complies with IP Complies with IP Complies with IP Complies with IP 0.03989 % 0.2975 % w/w 98.7 % OAB Claim / Limit Off-white to light tan or light yellow powder; odourless. NMT 50 PPM NMT 0.3 % NMT 0.5% w/w 97.0% to 103.0%

OPINION : In the opinion of the undersigned, the sample referred to above is of standard quality as defined in the act and the rules thereunder with respect to the tests carried out and mentioned above as per IP-96.

Date

: 30/01/99

Analyst

Q.C. Incharge.

RAW MATERIAL : CARBOMER 934 PROTOCOL : USP

PAGE: 01 OF 04

Carbomer 934 is a high molecular weight polymer of acrylic acid cross-linked with allyl ethers of sucrose. Carbomer 934, previously dried in vacuum at 80 deg for 1 hour, contains not less than 56.0 percent and not more than 68.0 percent of carboxylic acid (-COOH) groups. The viscosity of a neutralised 0.5 percent aqueous dispersion of Carbomer 934 is between 30,500 and 39,400 centipoises. PACKAGING AND STORAGE : Preserve in tight containers. LABELLING : Label it to indicate that it is not intended for internal use. IDENTIFICATION :A. Prepare a 1 in 100 dispersion of it To one portion of the dispersion add thymol blue TS: an orange color is produced. To another portion of the dispersion add cresol red TS: a yellow color is produced. Adjust a 1 in 100 dispersion of it with 1 N sodium hydroxide to about Ph 7.5: a very viscous gel is produced.

B.

RAW MATERIAL : CARBOMER 934 PROTOCOL : USP

PAGE : 02 OF 04

VISCOSITY ; (911) Carefully add 2.5 gm , previously dried in vacuum at 80 deg for 1 hour, to 500 ml of water in a 1000 ml beaker, while stirring continuously at 1000 +/- 10 rpm, with the stirrer shaft set at an angle of 60 deg and to one side of the beaker , with the propeller positioned near the bottom of the beaker. Allow 45 to 90 seconds for the addition of the test preparation at a uniform rate, being sure that loose aggregates of powder are broken up, and continue stirring at 1000 +/- 10 rpm for 15 minutes. Remove the stirrer, and place the beaker containing the dispersion in a 25 +/- 0.2 deg water bath for 30 minutes. Insert the stirrer to a depth necessary to ensure that air is not drawn into the dispersion, and while stirring at 300 +7- 10 rpm, titrate (see Titrimetry (541) with a calomel-glass electrode system to a pH of between 7.3 and 7.8 by adding sodium hydroxide solution (18 in 100) below the surface, determining the end point potentiometrically. The total volume of sodium hydroxide solution (18 in 100) used is about 6.2 ml . Allow 2 to 3 minutes before the final pH determination. [ Note — If the final pH exceeds 7.8, discard the mucilage , and prepare another using a smaller amount of sodium hydroxide for titration ] Return the neutralized mucilage to 25 deg water-bath for 1 hour, then perform the viscosity determination without delay to avoid slight viscosity changes that occur 75 minutes after neutralization. Equip a suitable rotational viscometer with a spindle having a cylinder 1.47 cm in diameter and 0.16 cm high attached to a shaft 0.32 cm in diameter, the distance from the top of the cylinder to the lower tip of the shaft being 3.02 cm, and the immersion depth being 4.92 cm (No. 6 spindle). With the spindle rotating at 20 rpm, observe and record the scale reading. Calculate the viscosity , in centipoises, by multiplying the scale reading by the constant for the spindle used at 20 rpm. LOSS ON DRYING: (731)Dry it in a vacuum at 80 deg for 1 hour; it loses not more than 2.0 % of its weight.

in ug .2 deg. maintained at a temperature of 85 deg . Test preparation : Accurately weigh about 10 mg of carbomer into a suitable 10 ml serum-type vial.0 % PROCEDURE : . Dilute 10.8-m column packed with 0. the use of headspace apparatuses that automatically transfer the measured amount of headspace is preferable to handling heated syringes for injecting the heated specimen. and seal with a metal cap. and mix.0 ml of this mixture with water to 500 ml . flowing at a rate of 20 ml per minute.2 % phase G39 on support S7. inject rapidly 1. The carrier gas is nitrogen. seal the vial. . insert the stopper without delay. add water to volume. Chromatographic system : (see Chromatography (621) — The gas chromatograph is equipped with a flame-ionization detector and a 2-mm x 1. insert a tight rubber stopper. Using a 2 ml of gas syringe preheated in an oven at 100 +/.[ In the following chromatographic procedure.0 ml of the gaseous phase from each vial separately into the chromatograph.002% BENZENE: PAGE : 03 OF 04 Standard preparation : Transfer 5. then raised at the rate of 5 deg per minute to 150 deg. Treat and inject the Standard preparation as directed under procedure. and mix until homogeneous.RAW MATERIAL : CARBOMER 934 PROTOCOL : USP HEAVY METALS: Method II (231): 0. Pipet 5 ml of this solution into a suitable 10 ml serum-type vial. of benzene in the weight of specimen taken by the formula : ru/rs. and mix to dissolve the specimen. add 5 ml of water. and measure the peak response for benzene. and measure the peak responses for benzene. Calculate the quantify . for at least 30 minutes. The column temperature is maintained at 80 deg for 4 minutes. The injector and detector are maintained at temperatures of about 200 deg.] Immerse the vials up to the rim of the cap in a thermostatic bath.7 ul (5 mg ) of benzene to a 500 ml volumetric flask. The relative standard deviation for replicate injection is not more than 5.

COOH) group. of the specimen taken .02VN/W ). using calomel —glass electrode system. The weight of benzene found is not more than 0.25 N sodium hydroxide VS.25 N sodium hydroxide VS. are the responses obtained from the Test preparation and Standard preparation . after each addition of 0. W is the weight. with the propeller positioned near the bottom of the beaker. Calculate the carboxylic acid content as a percentage of carboxylic acid groups taken by the formula 100 (45. N is the normality of sodium hydroxide solution . in which V is the volume in ml. . before recording the pH. ASSAY FOR CARBOXYLIC ACID CONTENT : Slowly add about 400 mg previously dried and accurately weighed . and 45. to 400 ml of water in 1000 ml beaker.01 % of the weight of the specimen taken. while stirring continuously at about 1000 rpm. of sodium hydroxide consumed.RAW MATERIAL : CARBOMER934 PROTOCOL : USP PAGE : 04 OF 04 in which ru and rs. respectively. and continue stirring for 15 minutes.02 is the molecular weight of the carboxylic acid (. Allow 1 minute for mixing . with the stirrer shaft set at an angle of 60 deg and at the side of the beaker. and titrate potentiometrically with 0. Reduce the stirring speed. in mg.

N. : UIR 287/98-99 Pub. Date Dt of Receipt Dt of Completion Qty sampled : R10400 : Mar'1999 : ———: 23/03/99 .0 % -— 68. T. 28/03/99 : 2xl5g RESULTS OF ANALYSIS & PROTOCOLS OF TEST APPLIED AS PER USP Protocols Description Results Complies with USP Claim / Limit White. Mfg. the sample referred to above is of standard quality' as defined in the act and the rules thereunder with respect to the tests carried out and mentioned above as net USP Date : 28-03-99 Analysis Q. the pH of a 1 in 100 dispersion is 3. .No.68kg Manufacturer: Goodrich Supplier : Hemlin Chemicals Ch.5 % NMT 2. Lab.NO.NO.C. fluffy powder having a slight characte.R. B Viscosity Benzene Loss on drying Heavy metals Content ofcarboxylic acid Complies with USP Complies with USP 31060cps Test Passes 0.R.45 % Complies with USP 66.0 % Solubility Identification A.ristic odour. : UI/RM/279/989 Batch No. Incharge. Date Exp.TEST CERTIFICATE (THE DRUGS AND COSMETICS ACT 1940 AND THE RULES THEREUNDER FORM 39) Rawmaterial : Carbomer 934 USP Party : Universal Impex G. 30500 — 39400 cps NMT 0.68kg-22. hygroscopic.20. No./Dt : 22-03-99 A. : KK832KA459 Batch Size : lx22.11%ODB OPINION : In the opinion of the undersigned.0 % NMT 0.002 % 56.R.

C and D are carried out. colourless or almost colourless.1996 GLYCEROL Glycerin is propane.2. The infra-red absorption spectrum of the resulting solution. Test B and C may be omitted if test A and D are carried out. is concordant with the reference spectrum of glycerin (85 %) or with the spectrum obtained from glycerin (85 %) RS. .3-triol PAGE : 01 OF 04 CATEGORY: Lubricant. laxative.RAW MATERIAL : GLYCERIN PROTOCOL : IP . calculated with reference to the anhydrous substances. IDENTIIFCATION : Test A be omitted if test B. pharmaceutical aid (humectant) DESCRIPTION : Clear. STANDARDS: Glycerin contains not less than 98. SOLUBILITY: Miscible with water and with ethanol (95 %). slightly soluble in acetone. practically insoluble in ether and in fixed oils and volatile oils. odourless.4. very hygroscopic. syrupy liquid.0 per cent of C3H8O3. A : To 5 ml add 1 ml of water and mix carefully.0 per cent and not more than 101.1. Appendix 5. STORAGE: Store in tightly-closed containers.

Appendix 6.1996 B: PAGE : 02 OF 04 Mix 1 ml with 0.470 and 1. determined at 20° .2 ml of 0. .1 M sodium hydroxide is required to produced a pink colour.1 M hydrochloric acid and sufficient water to produce 25 ml.RAW MATERIAL : GLYCERIN PROTOCOL : IP . The solution is colourless and not more than 0.475.2 HEAVY METALS: Not more than 5 ppm. Appendix 6.5 ml of phenolphthalein solution. The solution is colourless. Appendix 8. the blue colour does not diffuse into the lower layer. IRON: 10 g complies with the limit test for iron.1.5 ml of potassium dichromate solution.0 g in 2 ml of 0. a blue ring develops at the interface of the two liquids. Appendix 3.13.5 ml of nitric acid and superimpose 0.12.0 % w/v solution in carbon-dioxide free water ( solution A) add 0.13 (4 ppm). Dilute 10 ml of solution A to 25 ml with water . determined by Method A on a solution of 4. between 1. Allow to stand for 10 minutes . Irritant vapours are evolved which blacken filter paper moistened with alkaline potassium mercuri-iodide solution. C: D: ACIDITY OR ALKALINITY: To 50 ml of a 50. Refractive index. Appendix 3. Reserve the final solution for the test for Ester CLARITY AND COLOUR OF SOLUTION : Solution A is clear. Heat 1 ml with 2 g of potassium hydrogen sulphate in an evaporating dish.

35 volumes of acetone and 10 volumes of ethanol (95%) as the mobile phase. . Not less than 8. using silica gel G as the coating substance and a freshly prepared mixture of 55 volumes of chloroform .1 M hydrochloric acid. close the flask and allow to stand for 1 hour.0 ml has been added and boil under reflux condenser for 5 minutes .1996 PAGE : 03 OF 04 CHLORIDE: 20 ml of solution A complies with the limit test for chlorides . The test is not valid unless the standard solution is pink.1 M hydrochloric acid is required to decolorise the solution. Cool. ESTER: Add 0. Solution (2) contains 0.1 M sodium hydroxide to the solution reserved in the test for Acidity or alkanity until a total of 10.5 ml of water and 1 ml of decolorised pararosaniline solution.10(25ppm). Apply separately to the plate 5 pi of each of the following solution. Appendix 3. add 0.15(30ppm). Appendix 3. SULPHATE: 10 ml of solution A complies with the limit test for sulphates . Appendix 4.5 ml of formaldehyde standard solution ( 5 ppm CH2O) in place of solution A.0 ml of 0. GLYCOLS AND RELATED SUBSTANCES : Carry out the method for thin-layer chromatography. ALDEHYDES AND REDUCING SUBSTANCES : To 7. Any color produced is not more intense than that obtained in a standard prepared at the same time and in the same manner but using 7.RAW MATERIAL : GLYCERIN PROTOCOL : IP .5 ml of phenolphthalein solution and titrate with 0.5 ml of solution A in a glass stoppered flask add 7.02 % w/v each ofdiethylene glycol RS. ethylene glycol RS and propylene glycol RS in ethanol (95 %) .0 % w/v solution of the substances being examined.6. Solution (1) is a 2.

add 25. me solution remains blue and no precipitate is produced. Appendix 3. Spray with a solution prepared by dissolving 1. mix and add dropwise 1 ml of freshly prepared copper sulphate solution. appendix 3.14 % solution of sodium periodate and 1 ml of 1 M sulphuric acid and allow to stand protected from light for 15 minutes. SUGARS : Heat 10 ml of solution A with 1 ml of 1 M sulphuric acid on a water bath for 5 minutes . determined on 5 g.24. determined on 1. allow it to dry in air for 1 hour. a clear blue solution is produced.0 ml of a 2. ASSAY: Weigh accurately about 0. allow to stand protected from light for 20 minutes and titrate with 0. Any secondary spot in the chromatogram obtained with solution (1) is not more intense than any of the spots in the chromatogram obtained with solution (2). mix throughly with 45 ml of water. Continue heating on the water-bath for 5 minutes. Perform a blank determination and make any necessary correction. SULPHATE ASH: Not more than 0.0 % w/w.22.1 % w/v solution of sodium metaperiodate and dry me plate in a current of warm air. Add 3 ml of 2 M Sodium hydroxide ( Carbonate-free).5 ml of phenolphthalein solution as indicator.00921 g of C3H8O . adding 50 ml of water followed by 20 ml of acetone and 10 ml of 0.8 g ofbenzidine in 50 ml of etfaanol (95 %).1996 PAGE : 04 OF 04 After removal of the plate. Allow the plate to dry in air.1 g. WATER: Not more than 2.2 M hydrochloric acid.1 M Sodium hydroxide is equivalent to 0. Add 5 ml of a 50 % w/v solution of ethylene glycol. Each ml of 0.RAW MATERIAL : GLYCERIN PROTOCOL : IP . spray with a 0.01 %.5 g.1 M sodium hydroxide using 0.

0 % to 101.0 kg. Manufacturer: ————— Supplier : Sneha chemicals Ch.01 % NMT 2. Protocols Description Results Complies with IP Claim / Limit Clear. Date Dt of Receipt Dt of Completion Qty sampled ——— ——— ——— 06/12/98 15/12/98 2 x 100 ml RESULTS OF ANALYSIS & PROTOCOLS OF TEST APPLIED AS PER IP -96. colourless.6141 % OAB NMT 0. Complies with IP Complies with IP D-1. Mfg.B. D Acidity & alkalinity Clarity & colour of sol. Heavy metals Iron Chloride Sulphate Aldehydes & Reducing sub.NO.470 to 1.C.NO. T.R.R.0 % OPINION : In the opinion of the undersigned.No*/Dt : Proforma / 02-12-98 A.96 Date : 15-12-98 Analyst Q. syrupy liquid.R.474 Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP 0.475 NMTSppm NMT 4 ppm NMT 25 ppm NMT 30 ppm Solubility Identification .C. very hygroscopic. Date Exp. 1.0% w/w 98. : E0804-14 Qty received : 1 x 250 kg. Incharge.TEST CERTIFICATE ( THE DRUGS AND COSMETICS ACT 1940 AND THE RULES THEREUNDER FORM 39 ) Rawmaterial : Glycerine IP Party : Universal Impex G. Lab. Esters Glycols & Related sub Sugars Sulphated ash Water Assay as C3H8O. odourless. : UIR 228/98-99 Pub.01996 % 0. . : UI/RM/223/989 Batch No.No. = 250.88499 % w/w 98.N. the sample referred to above is of standard quality as defined in the act and the rules thereunder with respect to the tests carried out and asestiened above as per IP-96 .

2-diol.RAW MATERIAL : PROPYLENE GLYCOL PROTOCOL : IP . with ethanol (95 %) . hygroscopic. practically odourless . Store in tightly-closed containers.75. colourless.1996 1. with acetone and with chloroform. CATEGORY : Pharmaceutical aid (humectant. SOLUBILITY : Miscible with water.09 DESCRIPTION : Clear. solvent) PAGE : 01 OF 04 MOL. WT .2-PROPANEDIOL C3 H8O Propylene glycol is (RS)-propane-l. . viscous liquid.

Appendix 6. Heat 0.5 ml of a 0.2. Appendix 8. a violet colour slowly appears.2 ml of a 3 % w/v solution ninhydrin in a 2.5 % w/v solution of sodium metabisulphite. acrid smell ofacrolein is perceptible. Add 1 ml to 0.RAW MATERIAL : PROPYLENE GLYCOL PROTOCOL IP STANDARDS: IDENTIFICATION : A.05 ml of 0.1.1 g of boric acid. The solution is greenish yellow and not more than 0. ACIDITY : Mix 10 ml with 40 ml of water and add 0.040.1 ml of bromothymol blue solution. a pleasant odour develops. PAGE: 02 OF 04 To 0. B. cool and add 0. CLARITY AND COLOUR: The substance being examined is clear.1 M sodium hydroxide is required to change the colour to blue.5 g of potassium bisulphate and heat gently. Appendix 6.01 % w/v solution . a fruity odour develops And when me solution is heated to dryness. Heat for 10 minutes on a water bath at 70 deg. Appendix 8. . and colourless. C.1 RELATIVE DENSITY: Between 1.035 and 1.15. no sharp.15 ml with 0. BOILING RANGE : Between 184 deg and 189 deg. cooled in ice add 5 ml of a cooled mixture of 10 ml of water and 90 ml of sulphuric acid.

2 ml of 0. me solution does not change its appearance within 5 minutes. REDUCING SUBSTANCES : Mix 1 ml with 1 ml of 6 M ammonia and heat in a water bath at 60 deg for 5 minutes.431 and 1. . the solution is not yellow. Use lead standard solution (Ippm Pb) to prepare me standard. added towards the end of the titration. as an indicator. determined by method D on 3 ml diluted to 12 ml with water.13.RAW MATERIAL : PROPYLENE GLYCOL PROTOCOL : IP REFRACTIVE INDEX: Between 1. Appendix 8. Not more than 0. Titrate the liberated iodine with 0. Immediately add 0. PAGE: 03 OF 04 HEAVY METALS: Not more than 5 ppm .1 M silver nitrate. Appendix 3.15 ml of 0.05 M sodium tmosulphate using 1 ml of starch solution .05 M sodium thiosulphate is required.12.433. OXIDISING SUBSTANCES : To 10 ml add 5 ml of water. 2 ml of potassium iodide solution and 2 ml of 1 M sulphuric acid and allow to stand in a ground-glass-stoppered flask protected from light for 15 minutes.

2 M hydrochloric acid. Allow to cool. After removal of the plate.1 % w/v solution of sodium metaperiodate and dry the plate in a current of warm air. Apply separately to the plate 5 ul of each of the following solutions.01 % w/w. adding 50 ml of water followed by 20 ml of acetone and 10 ml of 0.02 % w/v each of diethylene glycol RS. 35 volumes of acetone and 10 volumes of efhanol (95 %) as the mobile phase. determined by the following method. Solution (1) is a 2. Solution (2) contains 0. SULPHATED ASH : Not more than 0. determined on 5 g. Allow the plate to dry in air. moisten the residue with sulphuric acid and ignite. Spray with a solution prepared by dissolving 1.6. Appendix 3. allow it to dry in air for 1 hour. . and ignite.RAW MATERIAL : PROPYLENE GLYCOL PROTOCOL : IP PAGE: 04 OF 04 OTHER GLYCOLS: Carry out the method for thin layer chromatography. Heat 50 g until it bums. using silica gel G as the coating substance and a freshly prepared mixture of 55 volumes of chloroform. WATER : Not more than 0. repeat the operations. spray with a 0.24. Any secondary spot in the chromatogram obtained with the solution ( 1 ) is not more intense than any of the spots in the chromatogram obtained with solution (2).2 % w/w. Appendix 4. ethylene glycol RS and propylene glycol RS in ethanol (95 %).0 % w/v solution of the substance being examined.8 gm of benzidine in 50 ml of ethanol (95%) .

/ Dt : 1562 / 03-03-99 A.R.00145 %w/w 0. the sample referred to above is of standard quality as defined in the act and the rules thereunder with respect to the tests carried out and mentioned above as per IP-96 Date : 07-03-99 Analy Q. Boiling Range Relative Density Refractive Density Heavy metals Oxidising Substances Reducing substances Other Glycols Sulphated ash Water Results Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP 187°C 1.431 Complies with IP Complies with IP Complies with IP Complies with IP 0.14875% w/w Claim / Limit Clear.0 kg.01% w/w NMT 0.03820 1.R. : UI/RM/265/989 Batch No.431 to 1.C Acidity Clarity & colour of sol.C. : -—— Mfg. practically odourless hygroscopic.N. Date : ------Dt of Receipt : 06/03/99 Dt of Completion : 07/03/99 Qty sampled : 2 x 100 ml RESULTS OF ANALYSIS & PROTOCOLS OF TEST APPLIED AS PER IP-96 Protocols Description Solubility Identification . colourless.035 to 1.NO. Date : Feb' 1999 Exp. No.TEST CERTIFICATE ( THE DRUGS AND COSMETICS ACT 1940 AND THE RULES THEREUNDER FORM 39 ) Rawmaterial : Propylene glycol IP Party : Universal Impex G.040 1. =645. Manufacturer : Spic Organics Supplier : Sneha Chemicals Ch.R. Lab.B. T. : 11902071 Qty received : 3x215 kg.2 %w/w OPINION : In the opinion of the undersigned.A. No.NO.433 NMT0. viscous liquid. : UIR 272/99-2000 Pub. 184°C to 189 °C 1. Incharge: .

make alkaline with dilute ammonia solution. ALUMINIUM. in 3 parts of alcohol (90%).pellets or fused mass. the insoluble residue. boil. very soluble in boiling ethyl alcohol. DESCRIPTION: Dry. page 928. page 971 . SOLUBILITY: Soluble in 1 part of water. brittle and showing a crystalline fracture. ARSENIC : Not more than 4 ppm.5 per cent w/v solution of ammonium nitrate. calculated as KOH and not more man 4. AND MATTER INSOLUBLE IN HCL : Boil 5 g with 40 ml of dilute HCL . IDENTIFICATION : Gives the reactions characteristic of potassium. filter. and wash athe residue with 2. IRON.0 per cent of K2CO3.RAW MATERIAL : POTASSIUM HYDROXIDE PROTOCOL : IP-1966 KOH Caustic Potash.11 STANDARDS: Potassium hydroxide contains not less than 85 % of total alkali. Very deliquescent. and in about 2. white sticks. hard. weighs not more than 5 mg. PAGE : 01 OF 02 56. Strongly alkaline and corrosive. cool.5 parts of glycerin. after ignition to constant weight.

add 5 ml of barium chloride solution. add 1 drop of phenolpthalein solution and dilute ammonia solution dropwise to produce a faint pink colour. Add 2 ml of acetic acid and water to make 25 ml. the limit of heavy metals is 30 ppm. Each ml of 1 N hydrochloric acid.6 ml of nitric acid.06911 g of K2C03. used in the combined titration is equivalent to 0.5 g dissolved in water with the addition of 1. Heat to boiling.RAW MATERIAL : POTASSIUM HYDROXIDE PROTOCOL : IP-1966 PAGE : 01 OF 02 CHLORIDE: 0. and titrate with 1 N hydrochloric acid.5 ml of alcohol. SULPHATE: Dissolve 1 g in water with the addition of 4. and 3 ml of potassium antimonate solution and allow to stand. To the solution in me flask add bromophenol blue solution. the solution complies with limit test for sulphates. and dissolve in 25 ml of water. 1. . HEAVY METALS: Dissolve 1 g in a mixture of 5 ml of water and 7 ml of dilute HCL. and continue the titration with 1 N hydrochloric acid. using phenolphfhalein solution as indicator. page 931. SODIUM : To 3 ml of a 10 per cent w/v solution add 1 ml of water.5 ml of hydrochloric acid. STORAGE: KOH should be kept in a well closed container. no white crystalline precipitate or sediment is visible to the naked eye within fifteen minutes ASSAY: Weigh accurately about 2 g. used in the second titration is equivalent to 0.05611 g of total alkali. calculated as KOH. complies with the limit test for chlorides. Each ml of 1 N hydrochloric acid. page 931. page 930.

-50.486 % 1. Date : ———Dt of Receipt : 02/09/98 Dt of Completion : 06/09/98 Qty sampled : 2 x 20 g RESULTS OF ANALYSIS & PROTOCOLS OF TEST APPLIED AS PER IP-66 Protocols Description Results Complies with IP Claim / Limit Dry.TEST CERTIFICATE (THE DRUGS AND COSMETICS ACT 1940 AND THE RULES THEREUNDER FORM 39 ) RAW MATERIAL : POTASSIUM HYDROXIDE IP Party : Universal Impex G. white pellets or fused mass.C. Manufacturer : The National Che. No. : UIR 141/98-99 Pub. the sample referred to above is of standard quality as defined in the act and the rules thereunder with respect to the tests carried out and mentioned above as per IP-66 Date : 06-09-98 Anatyst Q. Cor Supplier : ———— Ch.NO. NMT: 5 mg NMT4PPM NMT 30 PPM NLT 85./Dt : 0037 / 98-99 A. very deliquescent. strongly alkaline & corrosive. . Incharge. Lab.394 % OPINION : In the opinion of the undersigned. : ——Qty received : lx50kg.NO. hard brittle and showing crystalline fracture.Date : -—— Exp. Iron & matter insoluble in HC1 Arsenic Chloride Heavy metals Sulphate Sodium Assay as KOH K2C03 Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP 85. : —-— Mfg.No.0kg.0% Solubility Identification Aluminium.N. : UI/RM/ Batch No.R.R. T.R.0 % NMT 4.

Dissolve 2 g in 25 ml of water. Appendix 5. SOLUBILITY: Soluble in water. CATEGORY: Pharmaceutical aid. IDENTIFICATION : A.0 per cent of CioHi4N2Na208. . 372.2H20. practically insoluble in chloroform and in ether. crystalline powder.RAW MATERIAL : DISODIUM EDETATE PROTOCOL : IP . 50 mg per kg of body weight. is concordant with the reference spectrum of disodium edetate or with the spectrum obtained from disodium edetate RS.2H2O PAGE : 01 OF 02 Mol. add 6 ml of lead nitrate solution. DESCRIPTION: White. Wt.4. The infra-red absorption spectrum. shake and add 3 ml of potassium iodide solution. upto a maximum of 3 g per day. DOSE : By intravenous injection. Make alkaline to red litmus paper with 2 M ammonia and add 5 ml of ammonium oxalate solution . sparingly soluble in ethanol (95%).5 % and not more than 101. B. no yellow precipitate is produced.1996 CioH14N2Na2O8. no preciptate is produced. STANDARD: Disodium Edetate contains not less than 98.24 Disodium Edetate is disodium ethylenediaminetetra acetate dihydrate. dictating agent in metal poisoning. odourless.

add 0. make alkaline to red litmus paper with 2 M ammonia and 3 ml of ammonium oxalate solution . Add 0. HEAVY METALS: Not more than 20 ppm.2.5.12. dissolve in sufficient water to produce 300 ml and add 2 g ofhexamine and 2 ml of 2M hydrochloric acid.0 and 5. Appendix 6.1.25 g of calcium chloride to each solution before adding mercaptoacetic acid. and colourless.1 M lead nitrate using about 50 mg of xylenol orange triturate as indicator. determined on 1. ASSAY: Weigh accurately about 0.0 % w/v solution in carbondioxide-free water is clear.11. .2H2O.0 g by Method A. Gives the reaction of sodium salts.RAW MATERIAL : DISODIUM EDETATE PROTOCOL : IP C. no precipitate is produced. Appendix 3.5 ml of a 10 % w/v solution of calcium chloride. Appendix 3. determined in a 5 % w/v solution. D.1 M lead nitrate is equivalent to 0. Appendix 8. Use 2 ml of lead standard solution (10 ppm Pb) to prepare the standard. Appendix 6. CLARITY AND COLOUR OF SOLUTION : A 5. 1996 PAGE: 01 OF 02 Dissolve 0. Each ml of 0.13 (80 ppm).5 g in 10 ml of water. pH: Between 4. Titrate with 0.03722 g of CioH14N2Na2O8.1.5 g. Appendix 3.5% w/v solution complies with the limit test for iron. IRON: 10ml of a2.

5 NMT 20 PPM NMT80PPM Bet. Date .—— Manufacturer: Alliance Dyechem P.R.2H2O Results Complies with IP Complies with IP Complies with IP 4. odourless Bet.C.L Dt of Receipt : 22/03/97 Supplier Smeeta traders Dt of Completion : 28/03/97 Ch.& D PH Clarity and colour of sol Heavy metals Iron Assay C10H14N2Na208.665 % Claim / Limit White. the sample referred to above is of standard quality as defined in the act & the rules thereunder with respect to the tests carried out & mentioned above as perJP—96 specifiction Date : 28/03/97 Analyst Q. Exp.0 and 5. Incharge .NO. crystalline powder. Lab.B. No. Date : ——. T. 4. =5. 98. : UI/RM/ Pub./Dt : 345/ 22-3-97 Qty sampled : 2x25g RESULTS OF ANALYSIS & PROTOCOLS OF TEST APPLIED AS PER IP -96.05989 % 100. July 96 Qty received : 1x5 kg. : 0116 Mfg.NO. : UIR 6/96-97 G.0% OPINION : In the opinion of the undersigned. : 0/A8888 Batch No.59 Complies with IP Complies with IP 0.No.5% and 101.0 kg.N. .TEST CERTIFICATE ( THE DRUGS AND COSMETICS ACT 1940 AND THE RULES THEREUNDER FORM 39 ) RAW MATERIAL : DISODIUM EDETATE IP Party : Universal Impex A.C.R. Protocols Description Solubility Identification A.R.

C and D may be omitted if test A and E are carried out. very slightly in water.RAW MATERIAL : METHYLPARABEN PROTOCOL : IP-1996 C8H8O3 Mol. Tests B. The infra-red absorption spectrum. is concordant with the reference spectrum of methylparaben or with the spectrum obtained from methylparaben RS. crystalline powder. D and E are carried out.0 per cent of C8H8O3.15 PAGE: 01 OF 03 Methyl Hydroxybenzoate Methyl paraben is methyl 4.C. A. in ether and in methanol. SOLUBILITY: Freely soluble in ethanol (95%).Wt.0 per cent and not more than 101. Appendix 5.l52. CATEGORY: Pharmaceutical aid ( antimicrobial preservative) DESCRIPTION : Colourless crystals or white. STORAGE: Store in well closed containers. .4. STANDARDS Methylparaben contains not less than 99. IDENTIFICATION : Test A may be omitted if test B.hydroxybenzoate.

CLARITY AND COLOUR OF SOLUTION : A 10 % w/v solution in ethanol (95%) is clear. add sufficient water to restore the original volume.1 M sodium hydroxide is required to change the colour of solution. D. Appendix 5. boil and add 0. Appendix 6. a precipitate is formed and the supernatant liquid becomes red. and not more intensely coloured than reference solution BYS6. Dissolve 0. CHLORIDE: Heat 2 g with 100 ml of water. PAGE : 02 OF 03 The light absorption in the range 230 to 360 nm of a 0. C.1 g in 2 ml of ethanol (95%). Boil 10 mg with 10 ml of water. ACIDITY: Dissolve 1. and filter. 0.1 ml of 0. 25 ml of the filtrate complies with the limit test for chlorides. Appendix 6. cool and add 0.2. cool.1 ml of bromocresol green solution. Appendix 3. Melts between 125° and 128°. absorbance at about 258 nm. a reddish violet colour is produced. Appendix 8. To 2 ml of the solution add 3 ml of ethanol (95%). .05 ml of ferric chloride solution.1. E.RAW MATERIAL : METHYLPARABEN PROTOCOL : IP-1996 B.8.52 to 0. Not more than 0.0 g in sufficient ethanol (95%) to produce 10 ml. 5 ml of carbon dioxide-free water and 0.56.5 ml ofmercuric nitrate solution.0005% w/v in ethanol (95%) exhibits a maximum at about 258 nm.5.10 (500 ppm).

added towards the end of the titration. dry it in a current of hot air and examine under ultra-violet light (254 nm).22.005072 g of C8H8O3. Appendix 4. Any secondary spot in the chromatogram obtained with solution (1) is not more intense than me spot in the chromatogram obtained with solution (2).0333 M potassium bromate is equivalent to half of the volume of 0. Cool and add 25.1 M sodium thiosulphate using 2 ml of starch solution.0333 M potassium bromate.0 ml of 0. no turbity is produced within 10 minutes. transfer to a glass-stoppered flask. as indicator. Add 15 ml of potassium iodide solution.5 % w/v solution of potassium bromide and 40 ml of glacial acetic acid.1%. 10 volumes of ethyl acetate and 2 volumes of anhydrous formic acid as the mobile phase. Appendix 3.02 % w/v respectively.RAW MATERIAL : METHYLPARABEN PROTOCOL : IP-1996 PAGE: 03 OF 03 SULPHATE: To 10 ml of the filtrate obtained in the test for chloride add 0. ASSAY: Weigh accurately about 80 mg.0333 M potassium bromate is equivalent to 0. The difference between the titrations represents the amount of potassium bromate required. 5 ml of a 12.1 ml of barium chloride solution. SULPHATED ASH: Not more than 0. Apply separately to the plate 5 ul of each of two solutions of me substance being examined in methanol containing (1) 2.15 ml of dilute hydrochloric acid and 0. immediately stopper the flask and allow to stand for 15 minutes.6. . Repeat the operation without the substance being examined. using silica gel HF254 as the coating substance and a mixture of 88 volumes of dichlormethane. add 25 ml of 2 M sodium hydroxide and boil gently under reflux condenser for 30 minutes. Each ml of 0. After removal of the plate.1 M sodium thiosulphate required for the titration. mix and titrate athe liberated iodine with 0. The volume of 0. RELATED SUBSTANCES: Carry out the method for thin-layer chromatography. add 10 ml of hydrochloric acid. cool in ice.0 % w/v and (2) 0.

R. T. 125°to 128° NMT 500 PPM NMT 0.03989 % 100. 0.542 E. Results Complies with IP Complies with IP Complies with IP C.R.C. 99. the sample referred to above is of standard quality. Incharge . C.C. =10.0% & 101. Date Aug' 2003 Dt of Receipt 17/10/98 Dt of Completion : 31/10/98 Qty sampled '2x20g RESULTS OF ANALYSIS & PROTOCOLS OF TEST APPLIED AS PER IP -96 Protocols Description Solubility Identification A. : UI/RM/167/989 Batch No. crystalline powder. Date . Sep'1998 Exp. 126° Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP 0.B.NO. : M/098/998 Qty received : 1x10 kg. Lab.1 % Bet. 0. : UIR 173/98-99 Pub. No.068 % Claim / Limit White. No.52 to 0.as defined in the act & the rules thereunder with respect to the tests carried put & mentioned above as get IP-96 specification Date : 31/10/98 Analyst Q. / Dt : 899 / 14-10-98 A.NO • ———— Mfg.0% OPINION : In the opinion of the undersigned.D & E Acidity Clarity and colour of sol Chloride Sulphate Related substances Sulphated ash Assay as C8H8O3.TEST CERTIFICATE (THE DRUGS AND COSMETICS ACT 1940 AND THE RULES THEREUNDER FORM 39 ) RAW MATERIAL : METHYL PARABEN IP Party : Universal Impex G.0 kg.R. Manufacturer : Salicylates & Chemical Supplier : Harish Enterprises Ch.N.56 E. odourless.

in ether and in methanol. in acetone. absorbance at about 258 nm.RAW MATERIAL : PROPYLPARABEN PROTOCOL : IP-1996 C10H12O3 Mol. The light absorption in the range 230 to 360 nm of a 0. crystalline powder.5. very slightly in water.44 to 0. Appendix 5. STORAGE: Store in well closed containers.47.20 PAGE: 01 OF 03 Propyi Hydroxybenzoate Propyi paraben is propyi 4.0 per cent of C10H12O3. Wt.0005% w/v in ethanol (95%) exhibits a maximum at about 258 nm. 180. SOLUBILITY: Freely soluble in ethanol (95%).hydroxybenzoate. 0.0 per cent and not more than 101. STANDARDS Propylparaben contains not less than 99. CATEGORY: Pharmaceutical aid ( antimicrobial preservative) DESCRIPTION : Colourless crystals or white. calculated with reference to the dried substance. . IDENTIFICATION: A.

RAW MATERIAL : PROPYLPARABEN PROTOCOL : IP-1996 B.1 ml of bromocresol green solution. Appendix 8. 5 ml of carbon dioxide-free water and 0. To 2 ml of the solution add 3 ml of ethanol (95%).15 ml of dilute hydrochloric acid and 0. Appendix 6. and not more intensely coloured than reference solution BYS6. C. Solution B is yellow to orange . CLARITY AND COLOUR OF SOLUTION : A 10 % w/v solution in ethanol (95%) is clear. no turbity is produced within 10 minutes.brown. cool. and filter.0 g in sufficient ethanol (95%) to produce 10 ml. CHLORIDE: Heat 2 g with 100 ml of water.1.2.10 (500 ppm). To a further 10 mg in a test tube add 1 ml of sodium carbonate solution. SULPHATE: To 10 ml of the filtrate obtained in the test for chloride add 0. Appendix 6.1 ml of barium chloride solution. add sufficient water to restore the original volume. Not more than 0. heat it to boiling for 30 seconds and cool (solution A). ACIDITY : Dissolve 1. Add at the same time to each of solution A and B 5 ml of aminophenazone solution and 1 ml of potassium ferricyanide solution and mix. Melts between 96° and 99°. Appendix 3. the substance partly dissolves (solution B).1 ml of 0. .8.1 M sodium hydroxide is required to change the colour of solution. Solution A is orange to red and the colour is clearly more intense than any similar colour that may obtained with solution B. PAGE : 02 OF 03 To about 10 mg in a test tube add 1 ml of sodium carbonate solution. 25 ml of the filtrate complies with the limit test for chlorides.

add 10 ml of hydrochloric acid. transfer to a glass-stoppered flask.5 % w/v solution of potassium bromide and 40 ml of glacial acetic acid. LOSS ON DRYING: Not more than 0. Apply separately to the plate 5 ul of each of two solutions of the substance being examined in methanol containing (1) 2.1 M sodium thiosulphate required for me titration. Each ml of 0. dry it in a current of hot air and examine under ultra-violet light (254 nm). Repeat the operation without the substance being examined. using silica gel HF254 as the coating substance and a mixture of 88 volumes of dichlormethane. Appendix 8.6.1%. as indicator. Appendix 4. ASSAY: Weigh accurately about 80 mg. mix and titrate athe liberated iodine with 0.6. SULPHATED ASH: Not more man 0. add 25 ml of 2 M sodium hydroxide and boil gently under reflux condenser for 30 minutes. Any secondary spot in the chromatogram obtained with solution (1) is not more intense than the spot in the chromatogram obtained with solution (2). Appendix 3.0333 M potassium bromate.5 %. 5 ml of a 12. immediately stopper the flask and allow to stand for 15 minutes.22. added towards the end of the titration.0333 M potassium bromate is equivalent to 0. Cool and add 25. .02 % w/v respectively.0333 M potassium bromate is equivalent to half of the volume of 0.1 M sodium thiosulphate using 2 ml of starch solution. cool in ice.RAW MATERIAL : PROPYLPARABEN PROTOCOL : IP 1996 PAGE: 03 OF 03 RELATED SUBSTANCES : Carry out the method for thin-layer chromatography. determined on 1 g by drying over silica gel for 5 hours.0 ml of 0.006007 g of C10H12O3. The volume of 0. 10 volumes of ethyl acetate and 2 volumes of anhydrous formic acid as the mobile phase.0 % w/v and (2) 0. Add 15 ml of potassium iodide solution. After removal of the plate. The difference between the titrations represents the amount of potassium bromate required.

crystalline powder.R. 99. A.44 to 0.47 E. Incharge .97° Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP 0.C. No.NO. Results Complies with IP Complies with IP Complies with IP A. odourless.1 % NMT0. Date : 1 x 10 kg.04% 0. Date : Salicylates & Chemical Dt of Receipt : Harish Enterprises Dt of Completion : 29/07/98 : 492/21-07-98 Qty sampled Party G.0. Protocols Description Solubility Identification A. / Dt UIR 98/98-99 : June' 1998 : May'2003 : 27/07/98 : 2xl0g RESULTS OF ANALYSIS & PROTOCOLS OF TEST APPLIED AS PER IP -96.07% Claim / Limit White. Qty received Manufacturer Supplier Ch. Batch No.0% OPINION : In the opinion of the undersigned.5% Bet.Lab.44% 100.NO : ——— : P/015/698 Mfg. the sample referred to above is of standard quality' as defined in me act & the rules thereunder with respect to the tests carried out & mentioned above as per IP—96 specifiction Date : 29/07/98 Analyst Q.N.0.452 C.TEST CERTIFICATE ( THE DRUGS AND COSMETICS ACT 1940 AND THE RULES THEREUNDER FORM 39 ) RAW MATERIAL : PROPYL PARABEN IP : Universal Impex A.0 kg.0%& 101. 96°to 99° NMT500PPM NMT 0.C Acidity Clarity and colour of sol Chloride Sulphate Related substances Sulphated ash Loss on drying Assay as C8H8O3. = 10. Exp. : : UI/RM/ Pub.TR.B.R. No.

add 0.02 Purified water is prepared by distillation by means of ion exchange or by any other appropriate means from suitable potable water mat complies with all relevant statutory regulations.1 ml ofbromothymol blue solution. colourless liquid. CATEGORY: Pharmaceutical aid (solvent) DESCRIPTION : Clear. STANDARD: ACIDITY OR ALKALINITY: To 10 ml.05 ml of methyl red solution.Wt. me resulting solution is not red. freshly boiled and cooled in a borosuicate glass flask. the resulting solution is not blue. To 10 ml add 0.RAW MATERIAL : PURIFIED WATER IP PROTOCOL : IP H2O 1996 PAGE: 01 OF 03 Mol. . odourless and tasteless. STORAGE: Store in well closed containers of a material that does not alter the properties of the water. 18.

1 ppm. HEAVY METALS: Not more than 0.01 M disodium edetate. In a glass evaporating dish evaporate 150 ml to 15 ml on a water bath.5 ml of the liquid being examined.5 ml of dilute ammonium chloride solution and 7. When viewed vertically the solution is not more intensely coloured than a solution prepared at the same time by adding 1 ml of alkaline potassium mercuri-iodide solution to a solution containing 2. . CALCIUM AND MAGNESIUM: To 100 ml add 2 ml of ammonia buffer pH 10. the appearance of the solution does not change for at least 15 minutes.0.12. 50 mg of mordant black II mixture and 0. Appendix 3.1 M silver nitrate.RAW MATERIAL : PURIFIED WATER IP PROTOCOL : IP-1996 AMMONIUM : PAGE: 02 OF 03 To 20 ml add 1 ml of alkaline potassium mercuri-iodide solution and allow to stand for 5 minutes.5 ml of 0. determined by Method D on 12 ml of a solution prepared in the following manner. a purple blue colour is produced. Use lead standard solution (1 ppm Pb) to prepare the standard .2 ml of 0. CHLORIDE: To 10 ml add 1 ml of 2 M nitric acid and 0.

02 M potassium permanganate and boil for 5 minutes .1 ml of barium chloride solution. OXIDISABLE SUBSTANCES: To 100 ml add 10 ml of 1 M sulphuric acid and 0. The residue weighs not more than 1 mg (0. dropwise with shaking.1 ml of diphenylamine solution and.1 ml of 0. 5 ml of sulphuric acid.1 ml of 2 M hydrochloric acid and 0. . Any blue colour in the solution is not more intense than that in a solution prepared at the same time and in the same manner using a mixture of 4.001 %). 0.RAW MATERIAL : PURIFIED WATER IP PROTOCOL • IP . SULPHATE: To 10 ml add 0.1996 NITRATE : PAGE: 03 OF 03 To 5 ml in a test-tube immersed in ice add 0.2 ppm). the solution remains faintly pink.5 ml of nitrate standard solution (2 ppm N03) (0.4 ml of 10 % w/v solution of potassium chloride. RESIDUE ON EVAPORATION: Evaporate 100 ml to dryness on a water-bath and dry to constant weight at 105°. Transfer the tube to a water-bath at 50° and allow to stand for 15 minutes. The appearance of the solution does not change for at least 1 hour.5 ml of nitrate-free water and 0.

: 12/98-99 Dt of Completion : 16/05/99 Qty sampled : Hit.2 ppm NMT 0.C.NO. Date : 16/05/98 Analyst Q. Dt of Completion : 16/05/99 RESULTS OF ANALYSIS & PROTOCOLS OF TEST APPLIED AS PER IP-96 Protocols Description Acidity or alkalinity Ammonium Calcium & magnesium Heavy metals Chloride Nitrate Sulphate Oxidisable matter Residue on evaporation Results Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP Complies with IP Claim / Limit Clear colourless liquid. odouless and tasteless. : PWR 12/97-98 Batch No.R. Incharge . NMT 0-1 ppm NMT 0.TEST CERTIFICATE (THE DRUGS AND COSMETICS ACT 1940 AND THE RULES THEREUNDER FORM 39 ) RAW MATERIAL : PURIFIED WATER IP Party : UniversalImpex A. the sample referred to above is of standard quality as defined in the act and the rules thereunder with respect to the tests carried out and mentioned above as per IP specifications.001% OPINION : In the opinion of the undersigned.

SECTION – IV DETAILS OF SPECIFICATIONS AND STANDARDS LAID DOWN BY THE MANUFACTURER FOR EACH PRODUCT TOGETHER WITH ITS METHOD OF ANALYSIS .

00 300.700 228/98-99 30.000 141/98-99 2.80% 0.2001 No 1 2 3 4 5 6 7 8 9 INGREDIENTS Piroxicam Carbomer 934 Glycerin Propylene glycol Potassium Hydroxide Disodium Edetate Methyl Paraben Propyi Paraben D. OF STARTING : 22/4/99 DT OF COMPLETION : 27/4/99 A. BY CH K BY LABEL CLAIM % w/w 0.400 6/96-97 0.DATE : MAR.000 272/98-99 60.0 — — — — — STORES INCHARGE PRODUCTION INCHARGE QUALITY CONTROL INCHARGE A.PeerbhoyBldg. .000 60.120 0.575 8/99-2000 287/98-99 2.575 1. : MF/UI-02 SR.50% 0. N0 :23 PACK SIZE :30GM DT.00 0 WT.120 300.to SPEC IP USP IP IP IP IP IP IP IP UNIVERSAL IMPEX 89.90 % 10.WaterQ.NO. ACTUAL 257/98-99 1. 1999 EXP. UIR QTY IN KGS THEOR.R NO.030 173/98-99 0.04% OVER AGES % w/w 5.700 2. Mumbai-400002 India MFC.M.16% 0.DATE : APR.01% 0.030 0.480 98/98-99 0.00% 0.400 2.S. .000 30.00% 20.. : 01 BATCH SIZE : 300 KGS MFG.480 0.RAW MATERIAL REQUISITION PRODUCT :ROXICAMGEL BATCH NO.

.. 1 2 3 4 5 6 DESCRIPTION Main mixing vessel Mechanical Sifter Colloid Mul Homogenisor S.S Mechanical Works Precitech Industries CAPACITY 300 Kgs 1400 rpm 200 Kgs 25000 tubes per shift A.LIST OF VESSELS AND EQUIPMENT USED SR.. NO......S. Storage vessels Filling Machine MAKE Aerolite Industries Smitact Equipments Clit Industries Remi Industries S. .

... All equipments are cleaned and washed thoroughly. 2. No material of previously run material should stick to these. 1. 7. All processing should be carried out under strict supervision of a Qualified Competent staff. Cleaning & General Instructions Ensure the following before commencing the production.. 5. 3. approval should be obtained from Quality Control Department after checking the wash water content.. : 01 BATCH SIZE : 300 KGS PAGE : 01 OF 03 A..MANUFACTURING PROCESS PRODUCT : ROXICAM GEL BATCH NO. Equipments and containers should be labelled at each and every stage of manufacturing. The floor and ceilings of the area should be thoroughly cleaned and should not contain any foreign material attached to it. The raw materials required must be previously checked for labels and weight. Production personnel should wear gloves and masks before they enter the manufacturing area while handling the material. 4. A. 6. Proper temperature records should be maintained throughout me processing as per the instructions... When machine is ready for use..

MANUFACTURING PROCESS PRODUCT : ROXICAM GEL BATCH SIZE : 300 KGS BATCH NO. Add carbomer -934 ( 2. Start heating and hold temp.480 Kgs) Propyi paraben (0.700 Kgs ) slowly with constant high speed stirring to form a uniform gel.00 Kg) by heating..... Continue stirring for 15-20 minutes and allow to stand over night. Temp.000 Kgs ) in a jacketted main mixing tank and start heating. Temp.55°C Checked By:. Continue stirring for 20-30 min.M water into the main mixing tank. of water phase :.000 Kgs ).120 kgs) in propylene Glycol (1. PREPARATION OF CARBOMER GEL. around 50 -55 ° C..__________ STEP III— Transfer 90 Lit of D.M. of water: __________ Checked By.. till solution is clear.. . Add the clear solution to STEP I. STEP II — Transfer 180 litres of D. STEP IV —In a separate container dissolve Methyl Paraben (0. Main Mixing Vessel cleaned by : Homogeniser cleaned by Checked by : : ____________ _____________ ________________ STEP I — Transfer Propylene Glycol ( 59.. Hold temperature around 55° C to 60° C. Checked by :A. Add disodium Edetate. : 01 PAGE : 02 OF 03 A. Water from STEP II to STEP I under high speed stirring. Glycerin ( 30. ___________ Note : Add Carbomer-934 into the vortex caused by high speed stirring.

Manufacturing Chemist : _____________ 4. to draw Sample ... Inform Q.. A.0).water (about 11 .575 kgs).S vessel from STEP I onto the main mixing tank under constant stirring and continue stirring for 30 min. Add Piroxicam (1.0) B. 2..S. Check pH (range 7.M.C. : 01 PAGE : 03 OF 03 STEP V — Add and dissolve potassium Hydroxide pellets (1. Manufacturing completed on : Date : _________ Time : _________ 7..M.. Make up the volume of the bulk.0 litres of D.00 kgs)> C.900 Kgs) in 6.00 kgs of D.. water. Manufacturing operator : _____________ 5. STEP VI — Transfer the contents of the S. . Transfer the bulk in the S. Start cooling.M.500 Kgs) in 6. DISSOLUTION AND ADDITION OF PIROXICAM : Add and dissolve potassium hydroxide (0. Stir well to get a clear solution.0 to 8. Filter and add to the main mixing tank and mix for about 20 minutes. Check pH (Range 7. Manufacturing started on : Date : ______ Time: ___________ 6. Storage vessel with proper label. Check for the theoretical yield : _________ 3. UNLOADING: 1.0 to 8. water.. by addition of remaining D. Filter and add to STEP I.PRODUCT : ROXICAM GEL BATCH SIZE : 300 KGS BATCH NO.

FILLING INSTRUCTION: Assemble the filling machine as per instruction.. A required information should be sent to Quality Control Department immediately after the commencement of the filling. Adjust the filling machine to get the desired weight. Only one product is to be filled at a time.. leakage . Wt. Quantity processing stage. Date and initials of the supervising authority.FILLING PROCESS A. 1. After the completion of filling or during online. the intimation should be given the packing department for packing. 1.. All the crates and machines should be labelled property indicating the product name.. Variation. 5. Single batch should start and finish at a time.. Batch No. All filled tubes should be transferred to the Packaging Department alongwith me transfer slip and complete records A..... FILLING IN-PROCESS : Check for parameters such as crimping. B. A filling chart should be maintained during the filling of the batch. coding. 3. 4. . 2. After getting the approval from Quality Control Department take the cream for filling. 3. 2. 4. 5. 6.

No. 2. Mfg . 1. SECONDARY PACKING : The outer cartons should be overprinted with Mfg.. Mfg. TERTIARY PACKING: The master shipper is formed with upper lids opened and the lower lids sealed by 3 inch BOPP tapes For 30 g :. 2.PACKING PROCESS A. Lie. Date & Retail price are given should be treated as a front side.. Thus 20 such outer are packed in one shipper. Finally the right hand side flaps on me carton should be folded and sealed. 1. Date. Exp Date & Retail price.. 3. Exp. Mfg. 2. Lie. One row consists of 5 x 2 outer. Date & Packing is pasted in the middle of the master shipper..... Batch No... The rows are placed vertically one after the another. The tube is carefully put in the carton by right hand holding the carton in the left hand. 4 in each row. Batch No. FOR 30 G : Twenty carton boxes are placed in 5 rows . No. Exp. An overprinted label with Product Name... The carton should be placed with inside tube in upright position. PRIMARY PACKING : The tube is packed in the carton from right hand side. Finally the opening flap is closed. Finally the master shipper is sealed by 3 inch BOPP tape with H type sealing to cover all end. The carton is unfolded and sealed from left hand side by the flaps.. Date. The side on which details ofMfg.. A. C. . B. Date. Batch No.The secondary outer are placed in two rows one above the another. 1.

NO.00 98. Chemist/Operators Quality Control Chemist A ………… .50 98.ANALYTICAL CHECKS PERFORMED DURING FILLING AND PACKING PROCESS SR.00 RESPONSIBILITY 1 2 Production In-Process Quality Control Mfg. 1 2 3 4 5 6 7 8 CHECKS Average weight Individual weight Coding Crimping Leak test Carton/Outer overprinting Shipper packing Labelling DURATION After every 30 min After every 60 min After every 30 min After every 30 min After every 30 min After every 30 min After every 30 min Each & every shipper THEORETICAL YIELD PROCESS Mixing Filling Packaging MINIMUM 99. .

0 to 15. The average net weight of the content of the 10 tubes is not less than labelled amount.. STANDARDS & ANALYTICAL CONTROL LIMITS DESCRIPTION: Yellow coloured homogeneous transparent gel. No significant leakages occur during or at the completion of the test in all samples . Select a sample of 10 filled tubes and remove any labelling. A. Clean and dry the exterior surfaces of the tube with absorbent cloth.. Thoroughly clean and dry the outside of the tubes by suitable means and weigh individually. IDENTIFICATION: pH: 7.. Dry and reweigh each empty tube along with its corresponding parts.. Difference between the two weights is the net weight of the content of the tube. ( Disregard traces of cream near the crimp or thread of the cap.0 to 8. MINIMUM FILL TEST: The average net weight of the content of the 10 tubes is not less than 15 g and the net weight of content of any of the tube is between 15. Quantitatively remove the content of each tube by cutting it open and washing with a suitable solvent. .. Place the tubes in a horizontal position on a sheet of filter in an oven maintained at 45°C ± 3°C for 8 hours. LEAICTEST: Limit: No leakage is observed in any of the 10 tubes tested.0 Determine directly on the cream using a suitable calibrated pH meter. Select 10 tubes of the gel with seal applied thoroughly..FINISHED PRODUCT : PROTOCOL : INHOUSE PAGE: 01 OF 02 FINISHED PRODUCTS SPECIFICATIONS.. if necessary taking care to retain the closure and other parts of each tube.5 g..

. 2. Further dilution were done as given under standard solution.... PROCEDURE : Measure the absorbance of acidic solution of both sample and standard at 326 nm using respective alkaline solution as blank and calculate the result by comparision.... . REAGENTS : 1.01 N methanolic hydrochloric acid.01 N methanolic sodium hydroxide PAGE : 02 OF 02 STANDARD SOLUTION: 10 mcg/ml of piroxicam in 0.01 methanolic hydrochloric acid and methanolic sodium hydroxide. SAMPLE SOLUTION : Accurately weighed quantity of the sample equivalent to 10 mg of the substance was extracted with methanol to get solution of 100 mcg/ml.FINISHED PRODUCT : ROXICAM GEL PROTOCOL : INHOUSE ASSAY: The method is based on differential spectroscopy. 0. 0. The method obeys Beer's law in the concentration range of 4-22 mcg/ml A..

SECTION – V CERTIFICATE OF STERILITY AND ABSENCE OF PROGEN : WHEREVER IT IS APPLICABLE .

SECTION – VI SAMPLES OF THE PRODUCT APPLIED FOR REGISTRATION IN THEIR ORIGINAL PACK .

The secondary outer are placed in two rows one above the another.. No.. PRIMARY PACKING: • • The tube is packed in the carton from right hand side. The rows are placed vertically one after the another.. Mfg . Exp.. Date.. Batch No. Date. Date & Packing is pasted in the middle of the master shipper. The carton is unfolded and sealed from left hand side by the flaps. An overprinted label with Product Name. Mfg. Mfg. Finally the master shipper is sealed by 3 inch BOPP tape with H type sealing to cover all end. Exp.. TERTIARY PACKING: The master shipper is formed with upper lids opened and the lower lids sealed by 3 inch BOPP tapes For 30 g :.SPECIFICATIONS OF THE PACKAGING MATERIAL A. Batch No. One row consists of 5 x 2 outer. Thus 20 such outer are packed in one shipper. The carton should be placed with inside tube in upright position. Lie. • • • . Date. The side on which details ofMfg. FOR 30 G : Twenty carton boxes are placed in 5 rows . The tube is carefully put in the carton by right hand holding the carton in the left hand. Date & Retail price are given should be treated as a front side. 4 in each row. B • • C. No. Exp Date & Retail price. Finally the right hand side flaps on the carton should be folded and sealed. Lie. Batch No. Finally the opening flap is closed. SECONDARY PACKING: The outer cartons should be overprinted with Mfg.

0 g (± . with proper impression of logo and readable printing in English language as per the art work.0mm ( ± 1 mm) 32.0mm (±lmm) 22. Both side open 145.SPECIFICATION FOR PACKING MATERIAL TUBES 30 G 1 Description Three colour tube . 120. (* The colour of the carton should match with the standard colour of the tube. (* The colour of the tube should match with the standard colour of the carton. with proper impression of logo and readable Printing in English language as per the art work.0mm (±lmm) 5.250 g) Should be complied as per IS specification Should be complied as per IS specification CARTONS 30 G 1 Description Three colour carton made out of 300 gsm Board.0mm (±lmm) 24. .0 mm ( ± 1 mm ) 137.0 mm ( ± 1 mm) 300 gsm (± 5 gsm ) 2 3 4 5 6 7 Length upto Shoulder Shoulder diameter Length upto cap Weight of empty tube Lacquering Porosity 2 3 4 5 6 Design Length Height Width Grammage A.

5 cm) 38. with proper impression of logo and readable printing in English language as per the art work. (* The colour of the outer should match with the standard colour of the tube & carton.5cm (±0.0cm (±0.SPECIFICATION FOR PACKING MATERIAL OUTERS FOR 30 G 1 Description Three colour Outer made out of 350 gsm Board . One side open 165.0mm (±lmm) Not less than 350 gsm 5 PLY SHIPPERS FOR 30 G 1 2 3 4 5 6 Description Design Length Height Width Grammage Five ply Master Shipper of 115 gsm each sheet.5 cm) 38.5cm (±0.0mm ( ± 1 mm ) 151. Both side open 54.5 cm) Not less man 575 gsm 2 3 4 5 6 Design Length Height Width Grammage .0mm (±lmm) 105.

SECTION .VII CERTIFICATE OF ANALYSIS .

00 to 8. 2.TEST CERTIFICATE ( THE DRUGS AND COSMETICS ACT 1940 AND THE RULES THEREUNDER FORM 39 ) Party Product Batch No.3564 35.0076 30. 7. ASSAY: Complies Ingredients Piroxicam IP Lab.5285 : : : : : A Pale yellow coloured homogenous gel.3890 35.5395 35. 4. : 0/C 11828 Qty drawn for sampling : 15x30g Packing details : 9878x 15g RESULTS OF ANALYSIS AND PROTOCOLS OF TEST APPLIED AS PER INHOUSE SPECIFICATION.47 Limit 7. Date Exp. Batch Size Mfg. Content % w/w contains 0.97 % OPINION : In the opinion of the undersigned.3856 5.5709 53741 Wt of net Content of Tube in G 30.0074 30.5347 5.3479 5.4701 35.5049 Percentage 100. : UIF 17/99-2000 Dt of the Receipt : 24/04/99 Dt of the Completion : 27/04/99 Public lab T.R.3849 35.NO. No DESCRIPTION IDENTIFICATION pH at 40°C LEAK TEST MINIMUM FILL TEST Wt of Filled Tube in g 35. the sample referred to above is of standard quality as defined in the act and the rules thereunder with respect to the tests carried out and mentioned above as per inhouse Specification Date : 27/04/99 Analyst Q.R.00 Complies Complies Sr No 6 7 8 9 10 Wt of Filled Tube in g 35.0% to 110.0048 30.4384 5.4427 35.0067 30. 5.0034 30.5766 353826 Wt of Empty Tube in g 5. Incharge.0043 30.0085 30.5 Limit : 90.0% Actual content % w/w contains 0.3782 5.4255 5. Positive for Piroxicam. .0057 30. 1. 3.4627 5.C.5322 Wt of Empty Tube in g 5.0085 1 2 3 4 5 Wt of net Content of Tube in g 30. No. Date : Universal Impex : Roxicam gel : 01 : 300 kgs : Apr'1999 : Mar'2001 A. A Pale yellow coloured homogenous gel.4331 35.0037 6.

SECTION .VII REFERENCE SAMPLES .

38% OAB . Date Exp.REFERENCE SAMPLES Ref. 2000 Aug 2005 0. Sample Batch No Manufacturer Mfg. Date Water Assay : : : : : : : Piroxicam IP PX – 028 / 200 Ramdev Chem Sept.098% w/w 99.

SECTION – IX BIOAVAILABILITY STUDIES .

SECTION – X SAFETY AND TOLERANCE STUDIES .

methyl and propyi hydroxybenzoates and purified water. The gel contained hypromellose. cetyl alcohol. methyl and propyi hydroxybenzoates and purified water. macrogol ointment. The modified hydrophilic bases contained white soft parrafin. triethanolamine.2 ) in the oil-in-water ointment basis was replaced by sodium bicarbonate-buffered solution (pH 9. sodium hydroxide. Drug release was adversely affected by inclusion of ethanol or macrogol 400. sodium lauryl sulphate. The general rank order of in. propylene glycol. . isopropyi lanolate. The gel basis (containing also dimethylsulphoxide) produced best in . The emulsion basis contained liquid paraffin. propylene glycol. stearic acid TP.BIOAVAILABILITY STUDIES Babar et al prepared gels and ointment bases containing piroxicam 1% in order to study the in-vitro release of the drug. stearyl alcohol. sodium hydroxide. in rabbits was superior to that from three other USP ointments ( Simple ointment. self emulsifying glyceryl monostearate. The relative bioavailabilities of two commercially available piroxicam 20 mg suppositories in dogs were found to be similar and greater than the oral bioavailability of a piroxicam capsule following administration of single doses of the preparation.vitro drug release both through me cellulose membrane and hair less mouse skin. methyl and propyi hydroxybenzoates and purified water. percutaneous absorbtion of piroxicam was increased. and petrolatum rose water ointment). glycerol.2).vitro drug release through a cellulose membrane from all bases evaluated was: gel basis>hydrophillic basis>emulsion basis. Marked inter individual and intra-individual difference in absorption were noted. The optimal effect was attained with the addition of 5 % urea. When the water (pH 7. sodium hydroxide. Tsai et al found that the percutaneous absorbtion of piroxicam from an oil-in-water ointment bases (university of California Hospital basis containing 12 % propylene glycol).

Increase the risk of stomach irritation. PREGENANCY: Contraindicated as it may affect the developing foetus. . To be used only under close medical supervision during last three months of pregnancy and lactation. ALCOHOL: Avoid . Products containing salicylates should be avoided or used with caution in patients with liver disease. BREAST FEEDING: Contraindicated as present in breastmilk & safety not established.SAFETY & TOLERANCE SPECIAL PRECAUTIONS It should not be applied over broken skin or wounds. OVER 60: Reduced dose necessary due to increased likelihood of adverse effects. vitamin K deficiency and before surgery. They are for external use only and contact with eyes or mucous membranes should be avoided. PAEDIATRICS : Not recommended in age below 6 years. pre-existing hypothrombinemia.

SECTION – XI DETAILED REPORTS COVERING PHARMACOLOGICAL ASPECTS TOXICOLOGICAL ASPECTS CLINICAL ASPECTS .

Enterohepatic recycling occurs. Piroxicam is well absorbed from the gastro-intestinal tract. . It is metabolised in the liver by hydrosylation and conjugation with glucuronic acid and excreted predominantly in the urine with smaller amounts in the faeces. Less than 5 % of the dose is excreated unchanged. peak plasma concentrations area reached 3 to 5 hours after oral dose.PHARMACOLOGICAL ASPECTS Piroxicam is a non-steroidal anti-inflammatory agent used in musculoskeletol and joint disorders . Piroxicam is extensively bound to plasma proteins (about 99%) and has a long plasma half-life of approximately 50 hours.

rash has occurred in patients taking piroxicam. paraesthesia and hair loss. pruritus. it would appear from the present evidence that the overall incidence of such reactions is not appreciably higher with piroxicam than with other non-steroidal anti. while the commonest side effects of piroxicam are indeed gastro-intestinal. Oedema. photosensitivity. 21: 707-10 EFFECT ON SKIN. EFFECTS ON THE ELECTROLYTES : Reversible hyperkalaemic hyperchloraemic acidosis in patients receiving piroxicam. Epigastric distress.TOXICOLOGICAL DATA ADVERSE EFFECTS The most frequent adverse effect occuring with Piroxicam are local irritation and erythema . tinnitus. Heartburn.inflammatory agents. have occurred in patients taking piroxicam. As with other NSAIDs. EFFECTS ON GASTRO-INTESTINAL TRACT . not previously recorded in the literature .Gerver D. . Nausea. However. Thrombocytopenia. skin rash. dermatitis. thrombocytopenic purpura and aplastic anaemia have been described in patients on piroxicam. In the past it has been suggested that piroxicam may have a higher incidence of gastrointestinal adverse effects than other NSAIDs. Seroius skin reaction attributed to piroxicam therapy include toxic epidermal necrolysis and pemphigus vulgaris. Vomiting. A report of the adverse reactions associated with piroxicam received by the Medicines Safety Centre in South Africa including two reactions. Adverse reaction of piroxicam. Phototoxic reactions have been described. EFFECTS ON THE BLOOD : Decrease in haemoglobin and haematocrit not associated with obvious gastro-intestinal bleeding. Drug intell din Pharm 1987 .

. Diuretics : Increased risk of renal damage. Corticosteroids. EFFECTS ON LIVER: A report of a patient who presented with features of acute hepatocellular injury after taking piroxicam 40 mg daily for 3 days. and acute intestinal nephritis have been associated with piroxicam. Monitor vital functions. Antihypertensives : reduces the beneficial effects pf piroxicam. Acute nephropathy with characteristic features of Henoch-Schonlein purpura. Gastric lavage. the liver disorder progressed to subacute hepatic necrosis and the patient died. Lithium : Incresed serum lithium. Aspirin : Reduces serum piroxicam. OVERDOSAGE mx Emesis. General supportive and symptomatic treatment. Activated Charcoal. acute renal failure.EFFECTS ON KIDNEYS . uraemia with hyperkalaemia. DRUG INTERACTION : Anticoagulants : Potentiation. oral anticoagulants and NSAIDs : Increased risk of bleeding.

vi. DURATION OF ACTION : Upto 2 days. Rheumatoid arthritisOesteoarthritis of superficial joints. ii. v. Postoperative pains Acute gout. iv. CHILDREN : Over 6 yr<15 kg : 5 mg OD. DOSAGE: ADULTS : Rheumatoid arthritis. OD Acute musculoskeletal disorder : 40 mg OD/BD for 7-14 days. ankylosing spondylitis. Gout : Over 4-5 days. 15-25 kg : 10 mg OD. vii. Some effects may last 7-10 days after the treatment has been stopped. periathritis & tendinitis. Acute musculoskeletal injuries. iii. Ankylosing spondylitis. osteoarthritis : 20 mg. Maintenance : 40 mg OD/BD for 4-6 days.PARTICULARS OF CLINICAL ASPECTS OF DRUGS INDICATIONS : i. Dysmenorrhoea. Arthritis : Full anti-inflammatory effect. OD. ONSET OF EFFECT : Analgesia : 3-4 hr. APPLICATION : Topical analgesic are to be applied to me affected area and rubbed lightly until the cream vanishes do not massage-do not apply bandages or heat on the affected areas following applications. Maintenance : 10-30 mg. . 26-45 Kg: 15mgOD.

SECTION – XII STORAGE DATA .

STORAGE DATA Piroxicam should be preserved in tight.4 that contained a 10-fold excess of the cyclodextrin. Hydroxyalkylated cyclodextrin derivatives were found to reduce the stability ofpiroxicam (0.5 mg in pH 7. light-rsistant containers Piroxicam gel should be Stored below 30°. stored at 21° to 71° .

No.97 % 27/4/99 12mth Ok 7. Mfg.0 Positive Piroxicam IP 0.R. . Date : UIFS 9/99-2000 : APR.5 % w/w Imth Ok 7.SHELF LIFE : STABILITY DATA REFERENCE SAMPLES FOR STABILITY TESTING The reference samples are picked from the hold store using the random sampling technique. Batch Size : Roxicam Gel : 01 : 300 kgs A.2001 Results of analysis & protocols of Test applied as per inhouse specification.42 % 30/4/2001 The samples are observed for any changes in physical properties after every three months and full analyticals testing is done after each year duration.4721 g = 94.0 to 8. They are kept on clean pallets in the stability room. OPINION: The product is stable for 24 months. Storage Condition : Store in cool dry dark place. 1999 : MAR.47 Ok 0.5049 g -100. Product Batch No.78 % 25/4/00 24mth Ok 7.20 Ok 0. Date Exp.35 Ok 0.4839 g =96. Test Stability Description PH Identification Assay Analyst Date Spec / Pharmacopeial Limit Pale yellow coloured homogenous gel 7.

Date : UIFS 13/99-2000 : MAY.31 Ok 0.4784 g = 95. Batch Size : Roxicam Gel : 02 : 300 kgs A.4941 g =98.5 % w/w Imth Ok 7. OPNION: The product is stable for 24 months.0 to 8.06 % 16/5/1999 12mth Ok 7.59 Ok 0. Storage Condition : Store in cool dry dark place. Mfg. They are kept on clean pallets in the stability room.2001 Results of analysis & protocols of Test applied as per inhouse specification.82 % 22/5/00 24 mm Ok 7. Test Stability Description PH Identification Assay Analyst Date Spec / Pharmacopeial Limit Pale yellow coloured homogenous gel 7.R. Product Batch No.No.0 Positive Piroxicam IP 0. 1999 : APR . Date Exp. .SHELF LIFE : STABILITY DATA REFERENCE SAMPLES FOR STABILITY TESTING The reference samples are picked from the hold store using the random sampling technique.46 Ok 0.5003 g =100.68 % 27/5/2001 The samples are observed for any changes in physical properties after every three months and fall analyticals testing is done after each year duration.

SECTION – XIII AUTHENTICATED PRICE LIST .

THE FOLLOWING IS THE AUTHENTICATED PRICE LIST SR.E. A B C D *E DESCRIPTION Ex-Factory Price Price to pharmacy in the country of origin Public price in the country of origin C I F price to U.A. main ports Export price (C I F ) to the neighbouring countries PRICE * Photo copy of Certificate (Authenticated) .

SECTION – XVI NAME OF THE COMPETITIVE DRUG MANUFACTURED BY OTHER FIRMS .

50 26.0% COMPANY BLUE CROSS IPCA PFIZER CIPLA SUNPHARMA TALENT LAB PACKING 30 gm gel 30 gm gel 15 gmgel 30 gm gel 30 gm gel 30 gm gel PRICE 28. .5 % FELCAM GEL 0.THE FOLLOWING ARE THE NAMES OF THE COMPETITIVE DRUG MANUFACTURED BY OTHER FIRMS.00 30. BRAND MINICAM GEL 0.5 % PANCAMGEL 1.20 26.00 1 29.5 % PIROX GEL 0.00 A.5 % DOLONEX GEL 0. .24 27.5 % MOVON GEL 0.

SECTION – XV OTHER COUNTRIES WHERE THE PRODUCT IS REGISTERED .

Photo copy of the certificate of registration of product in other country NOT REGISTERED IN OTHER COUNTRIES .

XVI DATE OF INTRODUCTION OF THE PRODUCT TO THE MARKET IN THE COUNTRY OF ORIGIN .SECTION .

You're Reading a Free Preview

Download
scribd
/*********** DO NOT ALTER ANYTHING BELOW THIS LINE ! ************/ var s_code=s.t();if(s_code)document.write(s_code)//-->