DRAFT LABEL

Rx

REICHNUT 60’s Tablets

Composition:
Each uncoated tablet contains
Vitamin A 1000 IU
Vitamin D 100 IU
Vitamin E 2IU
Thiamine 0.81mg
Riboflavin 1.0mg
Niacin 10.0mg
Pyridoxine 0.1 mg
Vitamin B12 0.5mcg
Calcium (Minimum) 2.5%
(Maximum) 3.5%
Phosphorus 2.5%
Potassium 0.4%
Salt (Minimum) 0.1%
(Maximum) 0.6%
Chloride 0.1%
Magnesium 0.15%
Iron 3.0mg
Copper 0.1 mg
Manganese 0.25 mg
Zinc 1.4 mg
Iron oxide black
Iron oxide red
Iron oxide red
Iron oxide yellow

VETERINARY NOT FOR HUMAN USE FOR TREATMENT OF ANIMALS ONLY

Mfg. Lic. No: 07/NG/AP/2013/F/G

Net Qty.:
Batch no.:
Date of Manufacture:
Date of Expiry:
MRP:

Manufactured by:
M/s. Reichindia Pharma Limited, Plot#51,TSIIC Industrial Park, Bhongir-508116.

Dosage:
Puppies and dogs under 10Ibs/4.54kg-1/2 tablet daily.
Dogs over 10Ibs/4.54kg-1tablet daily.

Storage : Store below 25°C Protect from light.

 MANUFACTURING PROCEDURE OF REICHNUT

1. DISPENSING: Dispense Raw materials &Lubricants as per BMR

2. SIFTING: Sifting of Mineral Premix30#, Pigment blend PB-86597 80#,Maize
starch150#,Lactose,Microcrystalline cellulose pass through 60#,Colloidal anhydrous
silica 20#,Pigment blend 80#,Vitamin premix 30#,Meat flavor, Magnesium stearate
pass through 60#.
3. BINDER PREPARATION: Take purified water and add starch to it to from starch
slurry free of lumps. Take remaining qty. of purified water in steam kettle heat to
boil. Add starch slurry to it under stirring to get translucent paste. Cool the paste to
60°C.
4. GRANULATION: Load the following materials in RMG & mix for 5 mins. Granulate
dry mix blend using binder solution of stage B.mix till proper wet mass is achieved. If
required, use additional purified water.
5. DRYING: Dry the wet mass in FBD at inlet temp.60°C till the LOD IS BETWEEN 2.0-
4.0 %(Checked at 105°C,for 5 mins).
6. SIZING: Size the granules through 20# sieve and mill the retention on a multilill
using 1.5mm screen, knives forward at medium /fast speed.
7. LUBRICATION: load the sized granules along with lubricants except magnesium
stearate in a Double cone blender & mix for 12 min at 10 RPM.
8. COMPRESSION: Compress the tablet as per the parameters. After compression
send sample for Analysis followed by Packing.
 REICHNUT
METHOD OF ANALYSIS

1) DESCRIPTION
(Requirement: Buff to brown coloured, mottled bone shaped, biconvex uncoated tablets
with parallel groove on both sides.)

Complies / does not comply

2) IDENTIFICATION:

For Vitamin A, Vitamin D & Vitamin E:

Mobile phase A: Prepare a filtered and degassed mixture of methanol and purified
water in the
ratio of 90:10

Mobile phase B: Acetonitrile

Chromatogram conditions:

Standard column: C18, 4.6mm x 25cm, 5 micron

Suitable column: Inertsil ODS column that contains packing C18, 4.6mm x 25cm, 5µ

Diluent: Methanol

Flow rate: 1.0ml/min

Detector: UV

Detector Wavelength: 280nm

Column oven temperature: 40C

Injection volume: 100µl

Mode: Gradient

Syringe rinse diluents: Methanol

Blank: Diluent

Gradient programme:

Time Mobile Mobile

phase A phase B

0 100 -
 15 100 -

25 10 90

35 5 95

60 5 95

65 100 -

70 100 -

(If necessary make suitable changes in the mobile phase)

Preparation of standard solution: Weigh accurately and transfer _______(about

40mg) of vitamin A acetate (previously melt at 60C) working standard into a 100ml
volumetric flask. Add sufficient amount of diluent. Sonicate to dissolve, cool and dilute
upto the mark with diluent. (Solution A)

Weigh accurately and transfer ________(about 60mg) of vitamin E acetate (oily) working
standard into a 100ml volumetric flask. Add sufficient amount of diluent. Sonicate to
dissolve, cool and dilute upto the mark with diluent. (Solution B)

Weigh accurately and transfer_______(about 50mg) of vitamin D3 working standard into a

250ml volumetric flask. Add sufficient amount of methanol. Sonicate to dissolve, cool and
dilute upto the mark with methanol. Further dilute 2ml to 100 ml with methanol. (Solution
C)

Further dilute 10ml solution A, 5ml of solution B and 1ml of solution C to a 100ml with
methanol.

Preparation of Composite sample: Weigh and crush 20 tablets and transfer the
crushed powder into an amber colored glass bottle with appropriate lids or self-sealing
polythene bag bearing composite sample for analysis’ label. Store at room temperature.

Preparation of sample solution: Weigh accurately a quantity of composite

sample_______(about 1g) of sample in 50ml volumetric flask. Add 3ml of purified water.
Shake to disperse the sample for 5 minutes. Heat in water bath at 60C for 5 minutes,
cool and add 35ml of methanol. Sonicate for 45 minutes, cool and dilute upto the mark
with methanol. Filter through 0.45µ syringe filter.

Procedure: Separately inject equal volume of each solution as per sequence of injection
into the chromatograph and record the peak area responses for the major peaks and
check for the system suitability requirements.

Observation: Observe the retention time of major peaks in the chromatogram of sample
preparation to that in standard preparation.
Observation:

Complies / does not comply

For Niacine, Pyridoxine, Riboflavin & Thiamine:

Mobile phase: prepare a filtered and degassed mixture of buffer and methanol in the
ratio of 75:25.

Buffer: Dissolve 4gm of sodium hexane sulphonate and 20ml of glacial acetic acid in the
ratio of 1500ml with purified water.

Chromatogram conditions:

Standard Column: C18, 4.6mm x 25cm, 5µm

Suitable Column: Peerless column that contains packing C18, 4.6mm x 25cm, 5µm

Diluent: Prepare a mixture of purified water, acetonitrile and glacial acetic acid in the ratio
94: 5: 1

Flow rate: 1.0ml/min

Injection volume: 20µl

Detector: UV

Wavelength: 270nm

Mode: Isocratic

Syringe rinse diluents: Water and Acetonitrile (70:30)

Blank: Diluent

Run time: About 43mins

(If necessary, make suitable changes in the mobile phase)

Preparation of standard solution: Weigh accurately _______(about 50mg) of thiamine

hydrochloride working standard into a 100ml volumetric flask. Add sufficient amount of
diluents. Sonicate to dissolve, cool and dilute upto the mark with diluent. (Solution A)

Weigh accurately_______(about 25mg) of pyridoxine hydrochloride working standard into

a 250ml volumetric flask. Add sufficient amount of diluents. Sonicate to dissolve, cool and
dilute upto the mark with diluents. (Solution B)
Weigh accurately ________(about 64mg) of Nicotinic and working standard into a 50ml
volumetric flask. Add sufficient amount of diluent. Sonicate to dissolve, cool and dilute
upto the mark with diluent. (Solution C)

Weigh accurately_______(about 30mg) of riboflavin working standard into a 100ml

volumetric flask. Add 2ml of 0.1M sodium hydroxide. Add sufficient amount of diluent.
Heat and sonicate for 5 minutes, cool and dilute upto the mark with diluent. (Solution D)

Further dilute 2ml of solution A, 2ml of solution B, 10ml of solution C and 5ml of solution
D to a 100ml with diluent.

Preparation of composite sample: Weigh and crush 20tablets and transfer the crushed
powder into an amber colored glass bottle with appropriate lids or self-sealing polythene
bag bearing ‘composite sample for analysis’ label. Store at room temperature.

Preparation of sample solution: Weigh accurately a quantity of composite

sample_______(about 1gm) of sample in 50ml volumetric flask. Add 2ml of 0.1M sodium
hydroxide. Add sufficient amount of diluent. Heat and sonicate for 30minutes, cool and
dilute upto the mark with diluent. Filter through 0.45µ syringe filter.

Procedure: Separately inject equal volume of each solution as per sequence of injection
into the chromatograph and record the peak area responses for the major peaks and
check for the system suitability requirements.

Observation: Observation the retention time of major peaks in the chromatogram of

sample preparation to that in standard preparation.

Complies / does not comply

For Vitamin B12:

Mobile phase A: Prepare a filtered and degassed mixture of purified water and glacial
acetic acid in the ratio of 750:10

Mobile phase B: Methanol

Chromatogram conditions:

Standard column: C18, 4.6mm x 25cm, 5µm

Suitable column: Inertsil ODS column that contains packing C18, 4.6mm x 25cm, 5µm

Injection volume: 500ml

Detector: UV

Detector wavelength: 361nm

Diluent: Purified water

Mode: Isocratic
Syringe rinse diluents: Purified water.

Blank: Diluent

(If necessary make suitable changes in the mobile phase)

Time Mobile Mobile Tempera Flow

(min) phase A phase B ture

0.00 87 13 25C 2.0

32.00 87 13 25C 2.0

40.00 77 23 25C 1.2

45.00 77 23 25C 2.0

50.00 5 95 50C 2.0

55.00 5 95 50C 2.0

60.00 87 13 25C 2.0

70.00 87 13 25C 2.0

Preparation of standard solution: Weight accurately and transfer_______(about

25mg) of Vitamin B12 working standard 50ml volumetric flask. Add sufficient amount of
purified water. sonicate to dissolve, cool and dilute upto the mark with purified water.
dilute 5ml to 50ml with purified water. Further dilute 2ml to 100ml with purified. Further
dilute 2ml to 20ml with purified water.

Preparation of sample solution: Weigh transfer _______(15gm) of sample in a 250 ml

beaker. Add 50ml of purified water. Sonicate for 30min with stirring, cool and transfer this
content to 100ml volumetric flask and dilute upto the mark with purified water.

Procedure: Separately inject equal volume of each solution as per sequence of injection
into the chromatogram and record the peak area responses for the major peaks and
check for the system suitability requirements.

Observation: Observe the retention time of peak in the chromatogram of sample

preparation to that in standard preparation.

Complies / does not comply

For Calcium, Phosphorous, Potassium, Chloride, Magnesium, Sodium:

Sample solution: Take _______(15gm) of sample in a 100ml beaker. Add 50ml of

purified water, sonicate for 10minutes with occasional stirring. Cool and transfer in 100ml
volumetric flask and dilute upto the mark with purified water. filter through whatman filter
paper No. 41. Use the solution for following tests.

For Calcium: To 5ml of solution, add 0.2ml of a 2% w/v solution of ammonia oxalate. A
white precipitate is produced which is only sparingly soluble in 6M acetic acid but is
soluble in hydrochloric acid.

Observation:

For Potassium: To 1ml of the sample solution, add 1ml of dilute acetic acid and 1ml of a
freshly prepared 10% w/v solution of sodium cobaltinitrite. A yellow or orange-yellow
precipitate is formed immediately.

Observation:

For Magnesium: To 2ml of sample solution, add 1ml of 6M ammonia. A white precipitate
is produced which is dissolved by adding 1ml of ammonium chloride solution. Add 1ml of
disodium hydrogen phosphate solution. A white crystalline precipitate is produced.

Observation:

For Sodium: To 2ml of sample solution, add 2ml of a 15%w/v solution of potassium
carbonate and heat to boiling. No precipitate is produced. Add 4ml of a freshly prepared
potassium antimonite solution and heat to boiling. Allow to cool in ice and if necessary
scratch the inside of the test tube with a glass rod. A dense, white precipitate is formed.

Observation:

For Phosphorous: To 2ml of sample solution, add 2ml of dilute nitric acid and 4ml of
ammonium molybdate solution and warm the solution. A bright yellow precipitate is
formed.

Observation:

For Chlorides: Acidify 2ml of sample solution, with dilute nitric acid, add 0.5 ml of silver
nitrite solution, shake and allow to stand. A curdy white precipitate is formed.

Observation:

For Iron & Zinc:

Sample stock solution: Weigh and transfer _______(about 15gm) of sample in a 100ml
beaker, add 50ml of purified water and 5ml of concentrated hydrochloric acid. Sonicate for
10minutes with occasional stirring.

Further transfer it into 100ml volumetric flask, dilute upto the mark with purified water.
Filter through whatman filter paper No. 41. Use this solution for test.
Test for Iron: To 1ml of sample stock solution, add 1ml of potassium ferricyanide
solution (5% solution). Observe for the precipitate.

Test for Zinc: To 5ml of sample stock solution, add 0.2ml of sodium hydroxide solution
(about 10M); a white precipitate is produced. Further add 2ml of sodium hydroxide
solution (about 10M); the precipitate dissolves. Then add 10ml of ammonium chloride
solution (10.7%w/v) and add 0.1ml of sodium sulphide solution (Dissolve with heating,
12gm of sodium sulphide in 45ml of a mixture of 10 volumes of water and 29 volumes of
glycerol (85%), allow to cool and dilute to 100ml with the same mixture (It should be
colourless). Observe for the precipitate

Complies / does not comply

For Copper & Manganese:

[Note: Internal standard (Internal standard mix of Agilent technologies part # 51 83-
4681) concentration should be 10ppb in each blank, sample, standard and spiked solution
to be analysed.]

Instrument details:

Instrument : Inductively coupled plasma mass spectroscopy (ICP-MS)

Make : Agilent technology

Model : 7500 series

Plasma conditions : 1. Plasma flow (15L/min)

2. Nebuliser pump speed (0.10 rps)

3. RF power (1500 watts)

Preparation of Standard solution: Use standard stock of 1000ppm solution of Ca, Fe,
P, K, Se, Mn, Cu, Zn, Cr, Mo, Mg, Na, Al, B, Co, Ni, Li, Cd, Hg, As, Pb, Zr.

From standard stock solution of 1000ppm solution in a 50ml centrifuge tube pipette 0.5ml
of each of Ca, Fe, P, K, Se, Mn, Cu, Zn, Cr, Mo, Mg, Na, Al, B, Co, Ni, Li, Cd, Hg, As, Pb,
Zr standard stock solution, add 2.5ml conc. HNO3 in it. Dilute up to 50.0ml with purified
water to get 10ppm mixed standard solution.

Take 1.0ml of above solution, add 0.5ml conc. HNO3 in it and dilute to 10.0ml with purified
water to get 1ppm mixed standard solution.

Take 1.0ml of above solution, add 0.5ml conc. HNO3 in it and dilute to 10.0ml with purified
water to get 100ppb mixed standard solution.

Using 100ppb, 1ppm and 10ppm mixed std solution, prepare following dilutions 1ppb,
10ppb, 20ppb, 50ppb, 100ppb, 200ppb, 500ppb, 1000ppb & 2000ppb.
Calibrate the instrument using these solutions prjor to analysis.

Preparation of standard blank solution: In a 15ml centrifuge tube 0.5ml conc. HNO3
dilute to 10.0ml with purified water.

Preparation of composite sample: Weigh and crush 20 tablets and transfer the crushed
powder into an amber coloured glass bottle with appropriate lids or self-sealing polythene
bag bearing ‘composite sample for analysis’ label. Store at room temperature.

Preparation of sample solution: Weigh accurately a quantity of composite sample

about 0.2gm of sample in a microwave digestion cell; add 6.0ml conc. HNO3 and 1.0ml
50% hydrogen peroxide solution in it and digest it in microwave digestor. After cooling
transfer it in a 50ml pp tube give washings and dilute it to 50ml with purified water.
(Aspirate this solution to determine copper & manganese.)

Preparation of sample blank solution: Take 6.0ml conc. HNO3 in a microwave digestion
cell add 1.0ml 50% hydrogen peroxide solution in it and digest it in the microwave
digestor. After cooling transfer it in a 50ml pp tube give washings and dilute it to 50ml
with purified water. (this solution is used as a blank for copper & manganese.)

Complies / does not comply

3) AVERAGE WEIGHT: Limit: 1.6000g ± 3% (1.5520 to 1.6480gm)

Determine on 20 tablets to be used for assay.

Wt of 20 tablets:

Avg wt:

Complies / does not comply

4) UNIFORMITY OF WEIGHT: Not more than two of the individual weight deviate
the average weight by more than ± 5.0% and none deviates by more than ±
10.0%

Determine on 20 tablets used for average weight

1 2 3 4 5 6 7 8 9 10

11 12 13 14 15 16 17 18 19 20
Complies / does not comply

5) HARDNESS: Not less than 7.0kgs/cm2

Determine on 10 tablets using suitable hardness tester

1 2 3 4 5 6 7 8 9 10

Complies / does not comply

6) FRIABILITY: NMT 1.00%w/w

Determine on10 tablets using circular friability apparatus.

Weight of 10 tablets:

After friability wt of 10 tablets

Loss:

Calculation: Before weight-after weight

Before weight

Complies / does not comply

7) Microbiological examination of non sterile products: Determined on 20gm of the

sample

Microbial enumeration tests:

Total aerobic microbial count: NMT 103cfu/gm

Total combined yeast and mould count: NMT 102cfu/gm

Test for specified microorganism:

E.coli: Should be absent per gm

Salmonelae: Should be absent per gm

Pseudomonas aeruginosa: should be absent per gm

Staphylococcus aureus: Should be absent per gm

Bile-Tolerant gram negative bacteria: NMT 102/gm

Complies / does not comply

8) Disintegration: Limit: NMT 30 minutes

Determine on 6 tablets using suitable disintegration test apparatus.

Result:

Complies / does not comply

 REICHNUT
FINISHED PRODUCT SPECIFICATION

S.No Test Limit

Description Buff to brown coloured, mottled bone shaped,
1. biconvex uncoated tablets with parallel groove on
both sides.

3. Avg. Wt of tablets 1.5520 to 1.6480gm

NLT 7.0 Kg/cm2

7. Hardness
NMT 1.0%
8. Friability