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Method for detecting dibenzothiazyl disulfide in cephalosporin drugs

A technology of dibenzothiazole disulfide and a detection method is applied in the directions of measuring devices, instruments, scientific instruments, etc., and can solve the problems of inability to effectively detect residual dibenzothiazole disulfide in cephalosporins, and achieves high accuracy, Low detection limit and good specificity

Pending Publication Date: 2022-06-28
BEIJING XINLINGXIAN MEDICAL TECH DEV CO LTD
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Problems solved by technology

[0007] The technical problem to be solved in the present invention is to provide a detection method capable of accurately measuring residual dibenzothiazole disulfide in cephalosporins, so as to overcome the inability of existing detection methods to effectively detect residual dibenzothiazole disulfide in cephalosporins Defects

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  • Method for detecting dibenzothiazyl disulfide in cephalosporin drugs
  • Method for detecting dibenzothiazyl disulfide in cephalosporin drugs
  • Method for detecting dibenzothiazyl disulfide in cephalosporin drugs

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Experimental program
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Embodiment 1

[0035] The detection operation process is as follows:

[0036] 1. Instruments and Reagents

[0037] Agilent 6470 LC / MS

[0038] Standard material: dibenzothiazole disulfide

[0039] Water: Watsons

[0040] Methanol: Chromatographically pure

[0041] Dioxane: Chromatographically pure

[0042] Phosphoric acid: analytical grade

[0043] Ammonia: 29.6%

[0044] 2. Chromatographic conditions:

[0045] Column: Agilent ZORBAX Eclipse 120EC-C18 3.0×50mm, 2.7μm

[0046] Mobile phase A: 0.5% formic acid in water

[0047] Mobile phase B: methanol

[0048] Flow rate: 0.4ml / min

[0049] Column temperature: 40℃

[0050] Diluent: Dioxane-phosphoric acid (85:15)

[0051] Elution gradient:

[0052] time (min) A(％) B(％) 0 25 75 8 10 90 8.01 25 75 11 25 75

[0053] 3. Mass Spectrometry Conditions

[0054] Scan Mode: MRM(+)

[0055] Interface: AJS-ESI

[0056] Drying gas flow rate: 5.0L / min

[0057] Drying gas temperature: 300℃

[0058] Sh...

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Abstract

The invention relates to a method for detecting dibenzothiazyl disulfide in cephalosporin drugs. The invention belongs to the field of drug impurity analysis and detection, and establishes a liquid chromatography-mass spectrometry detection method for accurately determining residual dibenzothiazyl disulfide in a drug in order to solve the problem that a vulcanization accelerator (dibenzothiazyl disulfide) is difficult to detect. The method is high in sensitivity and good in precision, and the detection quantitation limit can reach 0.03 ng / ml. The method is suitable for accurate determination of dibenzothiazyl disulfide in drugs, and provides reference for formulating related drug detection quality standards.

Description

technical field [0001] The invention belongs to the technical field of drug analysis and detection, in particular to a method for detecting residual dibenzothiazole disulfide in cephalosporins. [0002] technical background [0003] Dibenzothiazole disulfide, commonly known as vulcanization accelerator, English name is 2,2'-Dithiobis(benzothiazole), abbreviated as MBTS, chemical formula C 14 H 8 N 2 S 4 , is a pale yellow needle crystal with a molecular weight of 332.49. It is slightly soluble in benzene, dichloromethane, carbon tetrachloride, acetone, etc. at room temperature, but insoluble in water, ethyl acetate and alkali. [0004] Dibenzothiazole disulfide (MBTS) is the raw material for the synthesis of cephalosporin antibacterial drug precursor-AE active ester, which may remain in cephalosporin drugs. MBTS is a genotoxic impurity. According to the limit guidelines of EMA Committee on Medicinal Products for Human Use on genotoxic impurities and the maximum daily dos...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/32G01N30/34G01N30/54G01N30/72
CPCG01N30/02G01N30/32G01N30/34G01N30/54G01N30/72G01N2030/324Y02A50/30
Inventor 彭燕董颖
Owner BEIJING XINLINGXIAN MEDICAL TECH DEV CO LTD
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