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[使用液相色谱-电喷雾电离串联质谱法同时测定屠宰动物肌肉、肝脏和肾脏中的五种青霉素]

[Simultaneous determination of five penicillins in muscle, liver and kidney from slaughtered animals using liquid chromatography coupled with electrospray ionization tandem mass spectrometry].

作者信息

Hatano Kazuhiro

机构信息

Fukuoka City Institute for Hygiene and Environment: 2-1-34, Jigyohama, Chuo-ku, Fukuoka 810-0065, Japan.

出版信息

Shokuhin Eiseigaku Zasshi. 2003 Feb;44(1):1-6. doi: 10.3358/shokueishi.44.1.

Abstract

A simple and rapid method for the simultaneous determination of five penicillins (ampicillin, penicillin G, penicillin V, oxacillin and cloxacillin) in muscle, liver and kidney tissues using high-performance liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS) was developed. Mass spectral acquisition was done in the negative ion mode by applying selected reaction monitoring (SRM). The five penicillins were extracted with water, and the extracted solution was cleaned up on a C18 cartridge. Phenethicillin was added as an internal standard, and the extract was diluted with water for injection into the LC-ESI-MS/MS. The recoveries of the five penicillins were in the range of 77.3-99.8% from muscle, liver and kidney fortified at 10-250 ng/g. The detection limits for ampicillin were 6 ng/g in muscle and kidney and 15 ng/g in liver. For penicillin G and penicillin V, the detection limits were 2 ng/g in muscle and kidney and 5 ng/g in liver. For oxacillin and cloxacillin, the detection limits were 4 ng/g in muscle and kidney and 10 ng/g in liver. Twenty-three muscle, fourteen liver and twenty-two kidney samples from the markets were analyzed by this method. No penicillins were detected in any sample.

摘要

建立了一种使用高效液相色谱 - 电喷雾串联质谱法(LC - ESI - MS/MS)同时测定肌肉、肝脏和肾脏组织中五种青霉素(氨苄青霉素、青霉素G、青霉素V、苯唑西林和氯唑西林)的简单快速方法。通过应用选择反应监测(SRM)在负离子模式下进行质谱采集。五种青霉素用水提取,提取液在C18柱上净化。加入苯氧乙基青霉素作为内标,提取物用水稀释后注入LC - ESI - MS/MS。在肌肉、肝脏和肾脏中添加浓度为10 - 250 ng/g的五种青霉素的回收率在77.3 - 99.8%范围内。氨苄青霉素在肌肉和肾脏中的检测限为6 ng/g,在肝脏中的检测限为15 ng/g。对于青霉素G和青霉素V,在肌肉和肾脏中的检测限为2 ng/g,在肝脏中的检测限为5 ng/g。对于苯唑西林和氯唑西林,在肌肉和肾脏中的检测限为4 ng/g,在肝脏中的检测限为10 ng/g。用该方法分析了来自市场的23份肌肉、14份肝脏和22份肾脏样品。在任何样品中均未检测到青霉素。

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