Pyridoxine Hydrochloride BP

Pyridoxine Hydrochloride
General Notices
(Ph. Eur. monograph 0245)
C8H12ClNO3 205.6 58-56-0
Action and use
Vitamin B6.
Preparations
Pyridoxine Tablets
Vitamins B and C Injection
When vitamin B6 is prescribed or demanded, Pyridoxine Hydrochloride shall be
dispensed or supplied.
Ph Eur
DEFINITION
(5-Hydroxy-6-methylpyridine-3,4-diyl)dimethanol hydrochloride.
Content
99.0 per cent to 101.0 per cent (dried substance).
CHARACTERS
Appearance
White or almost white, crystalline powder.
Solubility
Freely soluble in water, slightly soluble in ethanol (96 per cent).
mp
About 205 °C, with decomposition.
IDENTIFICATION
First identification: B, D.
Second identification: A, C, D.
A. Ultraviolet and visible absorption spectrophotometry (2.2.25).
Solution A Dilute 1.0 mL of solution S (see Tests) to 50.0 mL with 0.1 M
hydrochloric acid.
Solution B Dilute 1.0 mL of solution A to 100.0 mL with 0.1 M hydrochloric acid.
Solution C Dilute 1.0 mL of solution A to 100.0 mL with the potassium dihydrogen
phosphate 0.025 M + disodium hydrogen phosphate 0.025 M solution described in
chapter 2.2.3.
Spectral ranges 250-350 nm for solution B; 220-350 nm for solution C.
Absorption maxima 288-296 nm for solution B; 248-256 nm and 320-327 nm for
solution C.
Specific absorbances at the absorption maxima:
— 425-445 for solution B at 288-296 nm;
— 175-195 for solution C at 248-256 nm;
— 345-365 for solution C at 320-327 nm.
B. Infrared absorption spectrophotometry (2.2.24).
Comparison pyridoxine hydrochloride CRS.
C. Thin-layer chromatography (2.2.27).
Test solution Dissolve 1.0 g of the substance to be examined in water R and dilute
to 10 mL with the same solvent. Dilute 1 mL of this solution to 10 mL with water R.
Reference solution Dissolve 0.10 g of pyridoxine
hydrochloride CRS in water R and dilute to 10 mL with the same solvent.
Plate TLC silica gel G plate R.
Mobile phase concentrated ammonia R, methylene
chloride R, tetrahydrofuran R, acetone R(9:13:13:65 V/V/V/V).
Application 2 µL.
Development In an unsaturated tank, over a path of 15 cm.
Drying In air.
Detection Spray with a 50 g/L solution of sodium carbonate R in a mixture of
30 volumes of ethanol (96 per cent) R and 70 volumes of water R; dry in a current
of air, spray with a 1 g/L solution ofdichloroquinonechlorimide R in ethanol
(96 per cent) R and examine immediately.
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.
D. Solution S gives reaction (a) of chlorides (2.3.1).
TESTS
Solution S
Dissolve 2.50 g in carbon dioxide-free water R and dilute to 50.0 mL with the same
solvent.
Appearance of solution
Solution S is clear (2.2.1) and not more intensely coloured than reference
solution Y7 (2.2.2, Method II).
pH (2.2.3)
2.4 to 3.0 for solution S.
Related substances
Liquid chromatography (2.2.29).
Test solution Dissolve 25 mg of the substance to be examined in water R and dilute
to 10.0 mL with the same solvent.
Reference solution (a) Dilute 1.0 mL of the test solution to 100.0 mL with water R.
Dilute 1.0 mL of this solution to 10.0 mL with water R.
Reference solution (b) Dissolve 2.5 mg of pyridoxine impurity A CRS and 2.5 mg
of 4-deoxypyridoxine hydrochloride R (impurity B) in water R and dilute to
10.0 mL with the same solvent. Dilute 2.0 mL of this solution to 10.0 mL
with water R.
Column:
— size: l = 0.25 m, Ø = 4.6 mm;
— stationary phase: base-deactivated end-capped octadecylsilyl silica gel for
chromatography R (5 µm).
Mobile phase Dissolve 2.72 g of potassium dihydrogen phosphate R in 900 mL
of water R, adjust to pH 3.0 with dilute phosphoric acid R and dilute to 1000 mL
with water R.
Flow rate 1.0 mL/min.
Detection Spectrophotometer at 210 nm.
Injection 5 µL.
Run time 2.5 times the retention time of pyridoxine.
Identification of impurities Use the chromatogram obtained with reference
solution (b) to identify the peaks due to impurities A and B.
Relative retention With reference to pyridoxine (retention time = about 12 min):
impurity A = about 1.7; impurity B = about 1.9.
System suitability Reference solution (b):
— resolution: minimum 1.5 between the peaks due to impurities A and B.
Limits:
— correction factor: for the calculation of content, multiply the peak area of
impurity B by 1.5;
— impurity B: not more than 1.5 times the area of the principal peak in the
chromatogram obtained with reference solution (a) (0.15 per cent);
— unspecified impurities: for each impurity, not more than the area of the
principal peak in the chromatogram obtained with reference solution (a) (0.10 per
cent);
— total: not more than twice the area of the principal peak in the chromatogram
obtained with reference solution (a) (0.2 per cent);
— disregard limit: 0.5 times the area of the principal peak in the chromatogram
obtained with reference solution (a) (0.05 per cent).
Loss on drying (2.2.32)
Maximum 0.5 per cent, determined on 1.000 g by drying in an oven at 105 °C.
Sulfated ash (2.4.14)
Maximum 0.1 per cent, determined on 1.0 g.
ASSAY
In order to avoid overheating in the reaction medium, mix thoroughly throughout
and stop the titration immediately after the end-point has been reached.
Dissolve 0.150 g in 5 mL of anhydrous formic acid R. Add 50 mL of acetic
anhydride R. Titrate with0.1 M perchloric acid, determining the end-point
potentiometrically (2.2.20). Carry out a blank titration.
1 mL of 0.1 M perchloric acid is equivalent to 20.56 mg of C8H12ClNO3.
STORAGE
Protected from light.

Pyridoxine Hydrochloride BP

Uploaded by

Copyright:

Available Formats

Pyridoxine Hydrochloride BP

Uploaded by

Document Information

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Pyridoxine Hydrochloride BP

Uploaded by

Copyright:

Available Formats

Pyridoxine Hydrochloride

You might also like

Pfad - The Proxy pFad of © 2024 Garber Painting. All rights reserved.