Valganciclovir hydrochloride impurity analytical detecting method

A valganciclovir hydrochloride and detection method technology, which is applied in the field of analysis and detection of valganciclovir hydrochloride impurities, can solve problems such as separation difficulties, and achieve the effects of high sensitivity, good linear relationship, and easy operation

Active Publication Date: 2015-07-01
HUBEI LIYI PHARM TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In order to solve the above technical problems, the present invention creatively adds a certain concentration of ammonium-containing formate or acetate into the mobile phase for the first ti

Method used

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  • Valganciclovir hydrochloride impurity analytical detecting method
  • Valganciclovir hydrochloride impurity analytical detecting method
  • Valganciclovir hydrochloride impurity analytical detecting method

Examples

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Embodiment 1

[0042] Chromatographic conditions: use phenylsilane bonded silica gel as filler, mobile phase is triethylamine ammonium formate buffer solution of pH=5.6 (contains three components triethylamine, ammonium formate and trifluoroacetic acid except water, its content Respectively: 0.2% (v / v) triethylamine, 0.05mol / L ammonium formate and an appropriate amount of trifluoroacetic acid, wherein an appropriate amount of trifluoroacetic acid is used to adjust the pH of the buffer to 5.6)-methanol, the The volume ratio of buffer to methanol is 95:5, the flow rate is 1.0ml / min, the detection wavelength is 254nm, the chromatographic column: COSMOSIL 5PE-MS 150×4.6mm, 5μm, the column temperature is 35℃, and the injection volume is 50μl.

[0043] Preparation of the test solution:

[0044] Get about 50mg of valganciclovir hydrochloride crude drug, accurately weighed, put in 100ml volumetric flask, add 0.001mol / L hydrochloric acid to dissolve and be diluted to scale, as valganciclovir hydrochl...

Embodiment 2

[0052] Chromatographic conditions: use phenylsilane bonded silica gel as filler, mobile phase is triethylamine ammonium acetate buffer solution (except water, containing three components triethylamine, ammonium acetate and formic acid, the contents of which are respectively : 0.25% (v / v) triethylamine, 0.03mol / L ammonium acetate and an appropriate amount of formic acid, wherein an appropriate amount of formic acid is used to adjust the pH value of the buffer solution to 5.3)-methanol, the buffer solution and methanol volume The ratio is 95:5, the flow rate is 1.0ml / min, the detection wavelength is 254nm, the chromatographic column: COSMOSIL 5PE-MS 150×4.6mm, 5μm, the column temperature is 35℃, the injection volume: 50μl.

[0053] Preparation of the test solution:

[0054] Take about 50 mg of valganciclovir hydrochloride crude drug, accurately weighed, put in a 100ml volumetric flask, add appropriate amounts of six impurities, and prepare guanine 5 μg / ml, ganciclovir 10 μg / ml a...

Embodiment 3

[0059] Chromatographic conditions: use phenylsilane-bonded silica gel as a filler, and the mobile phase is triethylamine ammonium acetate buffer solution of pH=5.4 (containing three components of triethylamine, ammonium acetate and trifluoroacetic acid except water, the content of which is Respectively: 0.35% (v / v) triethylamine, 0.03mol / L ammonium acetate and an appropriate amount of trifluoroacetic acid, wherein an appropriate amount of trifluoroacetic acid is used to adjust the pH of the buffer to 5.4)-methanol, the The volume ratio of buffer to methanol is 96:4, the flow rate is 1.0ml / min, the detection wavelength is 254nm, the chromatographic column: COSMOSIL 5PE-MS 150×4.6mm, 5μm, the column temperature is 30℃, and the injection volume is 50μl.

[0060] Preparation of the test solution:

[0061] Take valganciclovir hydrochloride tablets, grind finely, accurately weigh an appropriate amount (approximately equivalent to 50 mg of valganciclovir hydrochloride main drug) and ...

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Abstract

The invention belongs to the technical field of the analytical chemistry and in particular discloses a valganciclovir hydrochloride impurity HPLC (High Performance Liquid Chromatography) analytical detecting method, and more specifically, the invention relates to a method for analytically detecting guanine, ganciclovir, methoxymethylguanine, ganciclovir 1-N-methyl-valine, mono acetoxyl ganciclovir, mono chloro ganciclovir or a medicine or a preparation containing the above six impurities. A solution to be detected is filled in a high performance liquid chromatographic column taking phenylsilane bonded silica gel as a filling agent, a moving phase prepared by an amine-containing aqueous inorganic salt solution and a chromatographically pure organic solvent is adopted to wash and separate, and then ultraviolet analysis and detection is carried out. According to the method, ammonium acetate or ammonium formate with certain concentration is firstly added in the moving phase creatively, and difficult problems that the main peak and the impurity peak and the adjacent impurity peaks are separated difficultly are thoroughly solved, the operation is simple, the separation degree is high, the sensitivity is high, the accuracy is good, and no similar literature is reported through literature retrieval.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a method for analyzing and detecting valganciclovir hydrochloride impurities by HPLC, more specifically, to a method for analyzing and detecting guanine, ganciclovir, and methoxymethylguanine , ganciclovir 1-N-methyl valine ester, monoacetoxy ganciclovir, monochloroganciclovir or a drug or preparation thereof containing the impurities in the above 6. Background technique [0002] Valganciclovir hydrochloride raw materials may produce six main impurities during the synthesis process and during the placement of valganciclovir hydrochloride solid preparations, namely guanine, ganciclovir, and methoxymethylguanine , Ganciclovir 1-N-methyl valine ester, monoacetoxy ganciclovir, monochloroganciclovir. [0003] Above-mentioned 6 kinds of impurity, how much its content directly affects the quality of valganciclovir hydrochloride or its preparation, easily causes human body ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/34
Inventor 史自东刘俊陈龙洪华云周震李霞余玉静
Owner HUBEI LIYI PHARM TECH CO LTD
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