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通过气相色谱/电子捕获检测进行定量后,利用气相色谱/串联质谱法对牛或猪肝提取物中的磺胺噻唑、磺胺二甲嘧啶、磺胺氯哒嗪和磺胺二甲氧嘧啶进行身份确认。

Confirmation of identity by gas chromatography/tandem mass spectrometry of sulfathiazole, sulfamethazine, sulfachloropyridazine, and sulfadimethoxine from bovine or swine liver extracts after quantitation by gas chromatography/electron-capture detection.

作者信息

Matusik J E, Sternal R S, Barnes C J, Sphon J A

机构信息

Food and Drug Administration, Division of Contaminants Chemistry, Washington, DC 20204.

出版信息

J Assoc Off Anal Chem. 1990 Jul-Aug;73(4):529-33.

PMID:2211474
Abstract

Four sulfonamide veterinary drug residues were quantitated by electron-capture detection (ECD) after separation by gas chromatography (GC). The identities of sulfathiazole (ST), sulfamethazine (SM), sulfachloropyridazine (SCP), and sulfadimethoxine (SDM) were confirmed in bovine or swine liver residues by tandem mass spectrometry (MS/MS). Bovine or swine liver tissues were extracted by using either the Tishler or the Manuel-Steller cleanup. The methylated residues containing ST, SM, SCP, and SDM were separated by GC prior to MS/MS daughter ion analysis. Control tissue, control tissue fortified at 0.1 ppm, and incurred tissue residues at approximately 0.1 ppm were analyzed for these 4 sulfonamides. A Finnigan Model TSQ-46 operating in the chemical ionization mode was used to perform the MS/MS daughter ion experiments. The identities of all 4 sulfonamides were confirmed in a single GC/MS/MS analysis.

摘要

通过气相色谱(GC)分离后,采用电子捕获检测(ECD)对四种磺胺类兽药残留进行定量分析。通过串联质谱(MS/MS)在牛或猪肝残留中确认了磺胺噻唑(ST)、磺胺二甲嘧啶(SM)、磺胺氯哒嗪(SCP)和磺胺二甲氧嘧啶(SDM)的身份。使用Tishler或Manuel-Steller净化方法对牛或猪肝组织进行提取。在进行MS/MS子离子分析之前,通过GC分离含有ST、SM、SCP和SDM的甲基化残留。对对照组织、添加浓度为0.1 ppm的对照组织以及浓度约为0.1 ppm的实际残留组织进行这4种磺胺类药物的分析。使用在化学电离模式下运行的Finnigan Model TSQ-46进行MS/MS子离子实验。在一次GC/MS/MS分析中确认了所有4种磺胺类药物的身份。

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