A kind of 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 increasing the difficulty of measuring the content of pharmaceutical impurities, low detection limit, complex matrix of pharmaceutical raw materials, etc., and achieves improved sensitivity and accuracy, Improved recovery and pretreatment rates, and reduced matrix interference

Active Publication Date: 2020-08-07
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 an efficient, sensitive, high recovery, and low detection limit processing and analysis method for qualitative Quantitative detection of trace diisopropyl sulfate content in difficult gasification pharmaceutical raw materials (such as thymol)

Method used

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  • A kind of detection method of genotoxic impurity diisopropyl sulfate in medicine
  • A kind of detection method of genotoxic impurity diisopropyl sulfate in medicine
  • A kind of detection method of genotoxic impurity diisopropyl sulfate in medicine

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Experimental program
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Embodiment 1

[0053] The establishment of embodiment 1 detection method

[0054] (1) Sample pretreatment

[0055] Accurately weigh 0.1g ± 0.01g of thymol raw material, add 1mL of methanol to extract, vortex and oscillate at a high speed of 5000r / min for 10min, and pass the supernatant through a 0.45μm microporous membrane for triple series series four Stage 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 in methanol to 100 mL, and mix well to obtain a 100 μg / mL stock solution of diisopropyl sulfonate reference substance. Accurately measure 100 μL of diisopropyl sulfonate reference substance stock solution, dilute to 10 mL with methanol, and mix well to obtain a 1 μg / mL standard reference substance solution. Take 10 μL, 50 μL, 200 μL, 100 μL, 200 μL, 500 μL, 1000 μL of 1 μg / mL standard reference solution, add methanol to dilute to 1.0 mL, and obtain concentrations ...

Embodiment 2

[0086] The detection of embodiment 2 actual samples

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

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

[0089] sample name Diisopropyl sulfate content (mg / kg) sample 1 N.D. sample 2 N.D.

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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, in particular to a detection method for genotoxic impurity diisopropyl sulfate in medicine. Background technique [0002] At present, there are relatively few analytical methods for the impurity content of diisopropyl sulfate in pharmaceutical raw materials, and the matrix of the pharmaceutical raw materials itself is complex and has a high boiling point, especially for some difficult-to-vaporize drugs. Gasified drug raw materials are not suitable, because the drug raw materials that are difficult to gasify will stay in the injection port, pollute the ion source, and even block the shunt nozzle and cause damage to the instrument; secondly, the detection limit of gas chromatography reported in the prior art is relatively high. [0003] The chemical name of thymol is 2-isopropyl-5-methylphenol, also known as thymol, thymol, thymol. At room temperature, thymol is a colorless translucent crystal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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