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The detection method of the impurity of pravastatin sodium

A technology for the detection of pravastatin sodium, which is applied in the field of detection of impurities, can solve problems such as poor method reproducibility, short and fat peaks, irregular drift of retention time, etc., and achieve the effect of good reproducibility and good stability

Active Publication Date: 2020-07-10
瀚晖制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the chromatogram of the related substances of the test product of the JP16 standard, such as figure 1 As shown in the sample, the impurity peaks that elute late in the sample have wide peaks, short and fat peaks, and the theoretical plate number of the main component is low, so the gradient setting of the method is unreasonable
In addition, in this method, the retention time drifts irregularly and seriously, and the method reproducibility is poor.

Method used

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  • The detection method of the impurity of pravastatin sodium
  • The detection method of the impurity of pravastatin sodium
  • The detection method of the impurity of pravastatin sodium

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Embodiment 1

[0048] A detection method of impurities of pravastatin sodium, comprising:

[0049] The concentration of pravastatin sodium in the need testing solution (self-developed preparation) of pravastatin sodium is 1mg / ml, and the concentration of pravastatin sodium in the need testing solution (reference preparation) of pravastatin sodium is 1mg / ml. ml.

[0050] Chromatographic conditions: the chromatographic column is Ultimate XB-C18 chromatographic column 4.6×250mm, 5μm. By volume, water: pH7.0 phosphate buffer: acetonitrile = 50:30:20 is mobile phase A, by volume, water: pH7.0 phosphate buffer: acetonitrile = 10:30:60 For mobile phase B, carry out gradient elution to the reference substance solution of pravastatin sodium and the test solution of pravastatin sodium respectively for 50min, the flow rate is 1ml / min, the column temperature is 25°C, the detection wavelength is 238nm, and the injection volume is 10μl , were eluted according to the following gradient elution procedure: ...

Embodiment 2

[0065] The difference between the detection method of the impurity of this pravastatin sodium and embodiment 1 is only:

[0066] Use water: pH7.0 phosphate buffer: acetonitrile = 52:30:18 as the mobile phase A, follow the gradient elution procedure as follows:

[0067] When t=0min, mobile phase A is 100%, and mobile phase B is 0%;

[0068] When t=0min~10min, the mobile phase A is 100%→100%, and the mobile phase B is 0%→0%;

[0069] When t=10min~55min, the mobile phase A is 100%→0%, and the mobile phase B is 0%→100%;

[0070] When t=55min~55.1min, the mobile phase A is 0%→100%, and the mobile phase B is 100%→0%;

[0071] When t=55.1min~60min, the mobile phase A is 100%, and the mobile phase B is 0%;

[0072] When t=50min, the mobile phase A is 100%, and the mobile phase B is 0%. The result is as Figure 5 As shown, the separation between the main component peak and the impurities before and after the main component peak is obviously increased, but the baseline is ugly.

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Abstract

The invention provides a detection method for impurities of pravastatin sodium, belonging to the technical field of drug detection. The chromatographic conditions of the detection method are listed asbelow: in an Ultimate XB-C18 chromatographic column, water-phosphate buffer with a pH value of 7.0-acetonitrile at a volume ratio of (48-52) to 30 to (18-22) is taken as a mobile phase A, the water-phosphate buffer with the pH value of 7.0-acetonitrile at a volume ratio of 10 to 30 to 60 is taken as a mobile phase B, enabling the reference solution and test solution of the pravastatin sodium to be subjected to gradient elution for 50-60 min, in the period, enabling the percentage of the volume of the mobile phase B accounting for the total volume dose of mobile phases to be increased from 0%to 100%, afterwards, decreasing to 0% and then eluting for 4-5 min. In the chromatograms of relevant substances obtained by the detection method, the resolutions of a main component peak and impurities before and after the main component peak are both greater than 2, baseline separation can be achieved, the reproducibility is good, the impurities and pravastatin sodium samples are effectively separated and detected, and the quality of the pravastatin sodium is controlled.

Description

technical field [0001] The invention relates to the technical field of drug detection, and in particular to a method for detecting impurities of pravastatin sodium. Background technique [0002] Pravastatin sodium is a competitive reductase inhibitor of 3-hydroxy 3-methylglutaryl coenzyme A (HMG.CoA). It was successfully researched by Sankyo in Japan. It was first listed in Japan in 1989 and has been listed in the United States Pharmacopoeia , "European Pharmacopoeia" and "Japanese Pharmacopoeia" included. In China, pravastatin sodium was included for the first time in the 2015 edition of the Chinese Pharmacopoeia, and the included formulations include pravastatin sodium tablets and pravastatin sodium capsules, which are used to treat hyperlipidemia and familial hypercholesterolemia . [0003] The detection results of related substances of pravastatin sodium by the method provided by JP16 (Japanese Pharmacopoeia 16th edition) were basically consistent with the sample detec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 杜加秋陆常辉董福霞王文萍
Owner 瀚晖制药有限公司
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