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A kind of HPLC detection method of valganciclovir hydrochloride intermediate hydrolyzate isomer

A technology of valganciclovir hydrochloride and a detection method, applied in the field of drug analysis, can solve the problems of detecting the purity of four isomers of an intermediate hydrolyzate, unfavorable product quality control of enterprises, etc., and achieve a reliable analysis and detection method, Ease of development and production, and short analysis times

Active Publication Date: 2021-02-12
HUBEI LIYI PHARM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] After consulting a large number of Chinese and foreign literature and patents, there is no literature report on the detection of the purity of the four isomers of the intermediate hydrolyzate by high performance liquid chromatography, which is not conducive to the control of product quality by enterprises

Method used

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  • A kind of HPLC detection method of valganciclovir hydrochloride intermediate hydrolyzate isomer
  • A kind of HPLC detection method of valganciclovir hydrochloride intermediate hydrolyzate isomer
  • A kind of HPLC detection method of valganciclovir hydrochloride intermediate hydrolyzate isomer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The separation effect test of different chiral columns of embodiment 1

[0047] (1) Stationary phase: silica gel surface coated with chiral crown ether

[0048] Column: CR(+)4.6*150mm, 5um

[0049] Chromatographic instrument: Agilent 1200 high performance liquid chromatograph

[0050] Detector and wavelength: UV-254

[0051] Mobile phase: Perchloric acid aqueous solution at pH 1.0

[0052] Flow rate: 0.8ml / min

[0053] Injection volume: 5ul

[0054] Column temperature: 25°C

[0055] Preparation of the test solution:

[0056] L-hydrolyzate and D-hydrolyzate mixed reference substance solution: Accurately weigh about 5 mg of D-hydrolyzate reference substance and about 5 mg of L-hydrolyzate reference substance, put them in the same 10ml measuring bottle, add mobile phase to dissolve and dilute to scale, shake well.

[0057] Take 5 μl of the above solution and inject it into the liquid chromatograph, record the chromatogram, the result is as follows: figure 1 show...

Embodiment 2

[0100] The detection effect test of embodiment 2 different mobile phases and their proportions

[0101] Chromatographic conditions:

[0102] (1) Mobile phase: n-heptane-ethanol (70:30, v / v)

[0103] (2) Mobile phase: n-hexane-isopropanol (50:50, v / v)

[0104] (3) Mobile phase: n-hexane-n-butanol (50:50, v / v)

[0105] (4) Mobile phase: n-hexane-ethanol (75:25, v / v)

[0106] (5) Mobile phase: n-hexane-ethanol (65:35, v / v)

[0107] Chromatographic instrument: Agilent 1200 high performance liquid chromatograph

[0108] Column: IC 4.6*250mm, 5um

[0109] Detector and wavelength: UV-254

[0110] Flow rate: 1.5ml / min

[0111] Injection volume: 5ul

[0112] Column temperature: 35°C

[0113] Preparation of the test solution:

[0114] Diluent: n-hexane-ethanol (50:50, v / v).

[0115] L-hydrolyzate and D-hydrolyzate mixed reference substance solution: Accurately weigh about 5 mg of D-hydrolyzate reference substance and about 5 mg of L-hydrolyzate reference substance, put them...

Embodiment 3

[0123] The detection effect test of embodiment 3 different wavelengths

[0124] (1) Detection wavelength: UV-250

[0125] (2) Detection wavelength: UV-260

[0126] (3) Detection wavelength: UV-254

[0127] Chromatographic instrument: Agilent 1200 high performance liquid chromatograph

[0128] Column: IC 4.6*250mm, 5um

[0129] Mobile phase: n-hexane-ethanol (70:30, v / v)

[0130] Flow rate: 1.5ml / min

[0131] Injection volume: 5ul

[0132] Column temperature: 35°C

[0133] Preparation of the test solution:

[0134] Diluent: n-hexane-ethanol (50:50, v / v).

[0135] L-hydrolyzate and D-hydrolyzate mixed reference substance solution: Accurately weigh about 5 mg of D-hydrolyzate reference substance and about 5 mg of L-hydrolyzate reference substance, put them in the same 10ml measuring bottle, add diluent to dissolve and dilute to scale, shake well.

[0136](1) The retention time of the L-hydrolyzate in (1) is 13.197min, 15.090min, the minimum resolution between the four...

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Abstract

The invention belongs to the field of drug analysis, and specifically discloses an HPLC detection method for an enantiomer of a valganciclovir hydrochloride intermediate hydrolyzate. The method uses cellulose-tri(3,5-dichlorophenylamino Formic acid ester) bonded silica gel as a chiral chromatographic column with a mixed solution of alkanes and alcohols as the mobile phase, the column temperature is 20-40°C, the flow rate is 1.0-1.5ml / min, and the wavelength is 250-260nm . The invention realizes the effective separation of four isomers of valganciclovir hydrochloride intermediate hydrolyzate, has good detection result accuracy, high sensitivity, simple operation, low cost and short analysis time, and is valganciclovir hydrochloride The quality control of intermediate hydrolyzate provides guarantee.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to an HPLC detection method for hydrolyzate isomers of valganciclovir hydrochloride intermediates. Background technique [0002] Valganciclovir hydrochloride is a synthetic inhibitor of herpes virus DNA, developed by the Swiss company Roche, and first listed as a prescription drug in Sweden and Finland in 2010, for the treatment of giant cells in patients with acquired immunodeficiency syndrome (AIDS) Viral (CMV) retinitis and prevention of CMV infection in high-risk solid organ transplant patients. In March 2001, it was approved by the US FDA, and in May 2001 it was first launched in the US. A number of studies at home and abroad have shown that valganciclovir hydrochloride tablets have obvious pharmacological effects, novel mechanism of action, low toxicity, few adverse reactions, significant clinical efficacy, high patient compliance, and safe application. [0003] The intermediate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 柳旭余再丹刘俊邓亚萍邵振周震刘欣
Owner HUBEI LIYI PHARM TECH CO LTD
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