Detection method of genotoxic impurity diisopropyl sulfate in medicine

A technology of diisopropyl sulfate and a detection method, which is applied in the field of analysis and testing, can solve the problems of low detection limit, increase the difficulty of measuring the content of drug impurities, complex drug raw material matrix, etc., so as to improve the recovery rate and the pretreatment rate. , improve sensitivity and accuracy, reduce the effect of matrix interference

Active Publication Date: 2018-10-23
中科广化(重庆)新材料研究院有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The complex matrix of drug raw materials, especially the high boiling point and difficult gasification properties further increase the difficulty of determining the content of drug impurities. Therefore, it is necessary to establish a

Method used

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  • Detection method of genotoxic impurity diisopropyl sulfate in medicine
  • Detection method of genotoxic impurity diisopropyl sulfate in medicine
  • Detection method of genotoxic impurity diisopropyl sulfate in medicine

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0053] Example 1 Establishment of detection method

[0054] (1) Sample pretreatment

[0055] Precisely weigh 0.1g±0.01g of thymol raw material, add 1mL of methanol to extract, vortex and centrifuge at 5000r / min for 10min. The supernatant is passed through a 0.45μm microporous membrane, and then the supernatant is subjected to triple series connection. Grade rod liquid mass spectrometry (LC-MS / MS) analysis.

[0056] (2) Preparation of standard working solution

[0057] Accurately weigh 10.0 mg of diisopropyl sulfate, dissolve it with methanol to make the volume to 100 mL, and mix well to obtain a 100 μg / mL diisopropyl sulfonate reference substance stock solution. Precisely measure 100μL of the diisopropyl sulfonate reference substance stock solution, dilute to 10mL with methanol, and mix well to obtain a 1μg / mL standard reference substance solution. Take 1μg / mL standard reference solution 10μL, 50μL, 200μL, 100μL, 200μL, 500μL, 1000μL, add methanol to dilute to 1.0mL, and obtain the ...

Example Embodiment

[0086] Example 2 Detection of actual samples

[0087] Precisely weigh 0.1013g (Sample 1) and 0.1008g (Sample 2) of thymol APIs respectively into two centrifuge tubes, add 1.0mL methanol to each, and centrifuge at 5000r / min after vortexing. After separation for 10 minutes, the supernatant was passed through a 0.45 μm microporous filter membrane, and 5.0 μL of the liquid was taken for HPLC-tandem mass spectrometry detection according to the method established in Example 1. The detection results are shown in Table 6.

[0088] Table 6 Content of Diisopropyl Sulfate in Thymol Pharmaceutical Raw Materials

[0089] sample name

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Abstract

The invention discloses a detection method of a genotoxic impurity diisopropyl sulfate in a medicine. The detection method comprises dissolving a thymol drug raw material, carrying out extraction, carrying out centrifugal separation at a high speed to obtain a supernatant, and analyzing the supernatant through a triple tandem quadrupole high-performance liquid chromatography-mass spectrometer to detect the content of the genotoxic impurity diisopropyl sulfate in the thymol drug raw material. According to the detection method, a diisopropyl sulfate recovery rate is in a range of 90-110%, a standard deviation (RSD) is 2.33%, a detection limit is 1.74 micrograms/kilogram and a quantitation limit is 5.81 micrograms/kilogram. The method has a low detection limit, a high recovery rate, high sensitivity and good repeatability and can be used for detection of genotoxic impurity diisopropyl sulfate in pharmaceutical raw materials including drugs difficult to gasify.

Description

Technical field [0001] The invention belongs to the field of analysis and testing, and particularly relates to a method for detecting genotoxic impurity diisopropyl sulfate in medicine. Background technique [0002] At present, there are relatively few analytical methods for the content of diisopropyl sulfate impurities in pharmaceutical raw materials, and the raw materials themselves are complex and have high boiling points, especially for some drugs that are difficult to vaporize. The gas chromatography or GC / MS in the prior art is difficult to use. Vaporized pharmaceutical raw materials are not suitable, because difficult-to-vaporize pharmaceutical raw materials will stay in the injection port, contaminate the ion source, or even block the splitter nozzle and cause damage to the instrument; secondly, the detection limit of gas chromatography reported in the prior art is relatively high. high. [0003] The chemical name of thymol is 2-isopropyl-5-methylphenol, also known as thym...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 曾瑜刘瑞赖华杰陈晓丹马倩靳焘
Owner 中科广化(重庆)新材料研究院有限公司
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