Zinc chloride EUROPEAN PHARMACOPOEIA 11.

Reference solution (a). Dissolve 40 mg of N-acetyl-ε- Loss on drying (2.2.32) : maximum 1.0 per cent, determined
caprolactam R (impurity C) in water R and dilute to 100.0 mL on 1.000 g by drying in an oven at 105 °C.
with the same solvent.
ASSAY
Reference solution (b). Dilute 5.0 mL of reference solution (a)
to 100.0 mL with water R. Dissolve 0.400 g in 10 mL of dilute acetic acid R. Carry out the
complexometric titration of zinc (2.5.11).
Reference solution (c). Dissolve 20 mg of zinc acexamate
impurity A CRS in water R and dilute to 50.0 mL with the 1 mL of 0.1 M sodium edetate is equivalent to 40.98 mg
same solvent. of C16H28N2O6Zn.
Reference solution (d). Dissolve 40 mg of ε-caprolactam R STORAGE
(impurity D) in water R and dilute to 100.0 mL with the same In a non-metallic container.
solvent. Dilute 5.0 mL of this solution to 100.0 mL with
water R. IMPURITIES
Reference solution (e). To 20 mL of test solution (a), add 5 mL Specified impurities : A, B, C, D.
of reference solution (b), 5 mL of reference solution (c), 5 mL
of reference solution (d) and 0.4 mL of a 100 g/L solution of
phosphoric acid R, then dilute to 50 mL with the mobile phase.
Reference solution (f). To 5.0 mL of reference solution (c),
add 5.0 mL of reference solution (b), 5.0 mL of reference
solution (d) and 0.4 mL of a 100 g/L solution of phosphoric A. 6-(6-acetamidohexanamido)hexanoic acid,
acid R, then dilute to 50.0 mL with the mobile phase.
Column :
B. 6-aminohexanoic acid (6-aminocaproic acid),
– size : l = 0.25 m, Ø = 4.0 mm ;
– stationary phase : end-capped octadecylsilyl silica gel for
chromatography R (5 μm).
Mobile phase : mix 0.2 volumes of phosphoric acid R,
8 volumes of acetonitrile R1 and 92 volumes of water
for chromatography R, then adjust to pH 4.5 with dilute
ammonia R1. C. 1-acetylazepan-2-one (N-acetyl-ε-caprolactam),
Flow rate : 1.2 mL/min.
Detection : spectrophotometer at 210 nm.
Injection : 20 μL of test solution (b) and reference solutions (b),
(e) and (f).
Run time : 8 times the retention time of zinc acexamate. D. azepan-2-one (ε-caprolactam).
Elution order : zinc acexamate, impurity D, impurity A,
impurity C. 01/2008:0110
System suitability : reference solution (e) : corrected 9.0
– resolution : minimum 3.0 between the peaks due to zinc
acexamate and impurity D ; if necessary, adjust the mobile
phase to pH 4.7 with dilute ammonia R1.
Limits :
– impurity A : not more than the area of the corresponding ZINC CHLORIDE
peak in the chromatogram obtained with reference
solution (f) (2 per cent); Zinci chloridum
– impurities C, D : for each impurity, not more than 1.5 times
the area of the corresponding peak in the chromatogram ZnCl2 Mr 136.3
obtained with reference solution (f) (0.15 per cent) ; [7646-85-7]
– unspecified impurities : for each impurity, not more than
0.5 times the area of the peak due to impurity C in the DEFINITION
chromatogram obtained with reference solution (f) Content : 95.0 per cent to 100.5 per cent.
(0.05 per cent) ;
CHARACTERS
– sum of impurities other than A : not more than 5 times the
Appearance : white or almost white, crystalline powder or cast
area of the peak due to impurity C in the chromatogram
in white or almost white sticks, deliquescent.
obtained with reference solution (f) (0.5 per cent) ;
Solubility : very soluble in water, freely soluble in ethanol
– disregard limit : 0.5 times the area of the peak due to
(96 per cent) and in glycerol.
impurity C in the chromatogram obtained with reference
solution (f) (0.05 per cent). IDENTIFICATION
Iron : maximum 50 ppm. A. Dissolve 0.5 g in dilute nitric acid R and dilute to 10 mL
Atomic absorption spectrometry (2.2.23, Method I). with the same acid. The solution gives reaction (a) of
Test solution. Dissolve 1.25 g in 20 mL of a 200 g/L solution chlorides (2.3.1).
of cadmium- and lead-free nitric acid R and dilute to 25.0 mL B. 5 mL of solution S (see Tests) gives the reaction of zinc
with the same acid solution. (2.3.1).
Reference solutions. Prepare the reference solutions using TESTS
iron standard solution (20 ppm Fe) R, diluting with a 200 g/L
solution of cadmium- and lead-free nitric acid R. Solution S. To 2.0 g add 38 mL of carbon dioxide-free water R
prepared from distilled water R and add dilute hydrochloric
Source : iron hollow-cathode lamp. acid R dropwise until dissolution is complete. Dilute to 40 mL
Wavelength : 248.3 nm. with carbon dioxide-free water R prepared from distilled
Atomisation device : air-acetylene flame. water R.

4424 See the information section on general monographs (cover pages)

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EUROPEAN PHARMACOPOEIA 11.0
pH (2.2.3) : 4.6 to 5.5.
Dissolve 1.0 g in 9 mL of carbon dioxide-free water R, ignoring
any slight turbidity.
Oxychlorides. Dissolve 10.0 g in 10 mL of carbon dioxide-free
water R. The solution is not more opalescent than reference
suspension II (2.2.1). To 1.5 mL of the solution add 7.5 mL
of ethanol (96 per cent) R. The solution may become cloudy
within 10 min. Any cloudiness disappears on the addition of
0.2 mL of dilute hydrochloric acid R.
Sulfates (2.4.13) : maximum 200 ppm.
Dilute 5 mL of solution S to 15 mL with distilled water R.
Prepare the standard using a mixture of 5 mL of sulfate
standard solution (10 ppm SO4) R and 10 mL of distilled
water R.
Aluminium, calcium, iron, magnesium. To 8 mL of
solution S add 2 mL of concentrated ammonia R and shake.
The solution is clear (2.2.1) and colourless (2.2.2, Method II).
Add 1 mL of disodium hydrogen phosphate solution R. The
solution remains clear for at least 5 min. Add 0.2 mL of
sodium sulfide solution R. A white precipitate is formed and
the supernatant remains colourless.
Ammonium (2.4.1) : maximum 400 ppm.
Dilute 0.5 mL of solution S to 15 mL with water R.
ASSAY
Dissolve 0.250 g in 5 mL of dilute acetic acid R. Carry out the
complexometric titration of zinc (2.5.11).
1 mL of 0.1 M sodium edetate is equivalent to 13.63 mg
of ZnCl2.
STORAGE
In a non-metallic container.
01/2022:2164 and filter. To 5 mL of the filtrate add 2 mL of cupri-tartaric
ZINC GLUCONATE
Zinci gluconas
C12H22ZnO14,xH2O Mr 455.7 (anhydrous substance)
DEFINITION
Zinc D-gluconate.
Content : 98.0 per cent to 102.0 per cent (anhydrous substance).
It may be anhydrous or contain a variable quantity of water.
CHARACTERS
Appearance : white or almost white, hygroscopic, crystalline
powder.
Solubility : soluble in water, practically insoluble in anhydrous
ethanol and in methylene chloride.
IDENTIFICATION
A. Thin-layer chromatography (2.2.27).
Test solution. Dissolve 20 mg of the substance to be
examined in 1 mL of water R.
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Zinc gluconate
Reference solution. Dissolve 20 mg of calcium gluconate CRS
in 1 mL of water R, heating if necessary in a water-bath at
60 °C.
Plate : TLC silica gel plate R (5-40 μm) [or TLC silica gel
plate R (2-10 μm)].
Mobile phase : concentrated ammonia R, ethyl acetate R,
water R, ethanol (96 per cent) R (10:10:30:50 V/V/V/V).
Application : 1 μL.
Development : over 3/4 of the plate.
Drying : at 100-105 °C for 20 min, then allow to cool to
room temperature.
Detection : spray with a solution containing 25 g/L of
ammonium molybdate R and 10 g/L of cerium sulfate R
in dilute sulfuric acid R, and heat at 100-105 °C for about
10 min.
Results : the principal spot in the chromatogram obtained
with the test solution is similar in position, colour and size
to the principal spot in the chromatogram obtained with
the reference solution.
B. Dissolve 0.1 g in 5 mL of water R. Add 0.5 mL of potassium
ferrocyanide solution R. A white precipitate is formed that
does not dissolve upon the addition of 5 mL of hydrochloric
acid R.
TESTS
Solution S. Dissolve 0.50 g in water R and dilute to 25 mL
with the same solvent.
Appearance of solution. Solution S is not more opalescent
than reference suspension II (2.2.1) and not more intensely
coloured than reference solution Y6 (2.2.2, Method II).
Sucrose and reducing sugars. Dissolve 0.5 g in a mixture of
2 mL of hydrochloric acid R1 and 10 mL of water R. Boil for
5 min, allow to cool, add 10 mL of sodium carbonate solution R
and allow to stand for 10 min. Dilute to 25 mL with water R
solution R and boil for 1 min. Allow to stand for 2 min. No
red precipitate is formed.
Chlorides (2.4.4) : maximum 500 ppm.
Dilute 5 mL of solution S to 15 mL with water R.
Sulfates (2.4.13): maximum 500 ppm.
Dissolve 2.0 g in a mixture of 10 mL of acetic acid R and 90 mL
of distilled water R.
Elemental impurities. Any method that fulfils the
requirements of general chapter 2.4.20. Determination of
elemental impurities may be used.
Element Maximum content (ppm)
Cadmium 1
Lead 2
Thallium 2
Water (2.5.32): maximum 12.0 per cent, determined on
80.0 mg.
ASSAY
Dissolve 0.400 g in 5 mL of dilute acetic acid R. Carry out the
complexometric titration of zinc (2.5.11).
1 mL of 0.1 M sodium edetate is equivalent to 45.57 mg
of C12H22ZnO14.
STORAGE
In a non-metallic, airtight container.
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