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Method for detecting toxic impurity DMAP in antibiotic drug raw materials

A detection method and antibiotic technology, applied in the field of analysis and testing, can solve the problems of high toxicity and irritation, damage to the respiratory system of the eyes, the nervous system of the digestive tract, and endanger human health, etc., and achieve the effects of low-cost detection, simple operation, and reliable results.

Active Publication Date: 2016-08-24
SHANDONG ANALYSIS & TEST CENT
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Problems solved by technology

However, DMAP itself is highly toxic and irritating, and can damage the eyes, skin, respiratory system, digestive tract, nervous system, etc., and endanger human health

Method used

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  • Method for detecting toxic impurity DMAP in antibiotic drug raw materials
  • Method for detecting toxic impurity DMAP in antibiotic drug raw materials
  • Method for detecting toxic impurity DMAP in antibiotic drug raw materials

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Embodiment Construction

[0024] The present invention will be further described below in conjunction with accompanying drawing.

[0025] Instruments and reagents

[0026] The main instruments used are: U3000 liquid chromatograph (Thermo Fisher Scientific Co., Ltd., USA), ABSCIEX5500 quadrupole tandem linear ion hydrazine mass spectrometer (QTRAP, American AB SCIEX company), Heraeus MultifugeX1R high-speed refrigerated centrifuge (Thermo Fisher Scientific Co., Ltd., USA), 10-100 μL pipette and 100-1000 μL pipette (Thermo Fisher Scientific Co., Ltd., USA), pH meter (Mettler-Toledo, Switzerland) .

[0027] The main reagents used are: chromatographic grade methanol (U.S. Aston Chemical Technology Co., Ltd.), chromatographic grade formic acid (U.S. ROE Technology Co., Ltd.), chromatographic grade acetonitrile (U.S. Aston Chemical Technology Co., Ltd.), analytically pure ammonium acetate ( Sinopharm Chemical Reagent Co., Ltd.), analytical pure acetic acid (Sinopharm Chemical Reagent Co., Ltd.), Wahaha dri...

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Abstract

The invention discloses a method for detecting the toxic impurity DMAP in antibiotic drug raw materials. The antibiotic drug raw materials are dissolved, diluted and centrifuged to obtain supernate, the supernate is subjected to high performance liquid chromatography-quadrupole series linear ion trap mass spectrum, and then the content of the toxic impurity DMAP in the antibiotic drug raw materials is detected. The mobile phase of high performance liquid chromatography is a mixture of ammonium acetate aqueous solution and acetonitrile solution. The mass-to-charge ratio (m / z) of the parent ion in quadrupole series linear ion trap mass spectrum for detecting DMAP is 122.7, and the mass-to-charge ratio (m / z) of the daughter ion is 107.1. The adopted pair of ions does not interfere with sample detection and is highest in response. By the adoption of the mobile phase, the retention time of a target compound on a chromatographic column can be prolonged, so that a detection result is more stable. The method is easy to operate, and the result is reliable. Quick and low-cost detection of the residual quantity of DMAP in the antibiotic drug raw materials can be achieved, and detection sensitivity can reach 0.50 mg / kg.

Description

technical field [0001] The invention belongs to the field of analysis and testing, and in particular relates to a detection method for toxic impurity DMAP in raw materials of antibiotic drugs. Background technique [0002] 4-dimethylaminopyridine (4-dimethylaminopyridine, DMAP), molecular formula such as figure 1 As shown, it is a new type of high-efficiency catalyst widely used in chemical synthesis in recent years. It can be used in the catalysis of various organic synthesis reactions such as acylation, alkylation, etherification, esterification and transesterification, and has a very obvious effect on improving the yield. Effect. The domestic chemical and pharmaceutical industry has successfully applied it to the production of antibiotic APIs such as propionylspiramycin, doripenem, and meropenem, improving the process conditions and achieving good economic and social benefits. However, DMAP itself is highly toxic and irritating, and can damage eyes, skin, respiratory sy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 王珊珊宁凡盛赵汝松苑金鹏陈跃
Owner SHANDONG ANALYSIS & TEST CENT
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