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液相色谱-串联质谱法测定蜂蜜中的链霉素残留量。

Determination of streptomycin residues in honey by liquid chromatography-tandem mass spectrometry.

作者信息

Granja Rodrigo H M M, Niño Alfredo M Montes, Zucchetti Roberto A M, Niño Rosario E Montes, Patel Raj, Salerno Alessandro G

机构信息

Microbioticos Laboratories, Av. Santa Isabel 2120, Campinas, SP, 13084-471, Brazil.

出版信息

Anal Chim Acta. 2009 Apr 1;637(1-2):64-7. doi: 10.1016/j.aca.2009.01.006. Epub 2009 Jan 10.

Abstract

Streptomycin is an aminoglycoside antibiotic used in apiculture to protect bees against a variety of brood diseases. Brazilian authorities have included it in the National Regulatory Monitoring Program for honey production. A simple and reliable method using liquid chromatography-tandem mass spectrometry has been developed and validated for the determination of streptomycin in honey. The chromatography separation was performed on a Gemini 5 microm C18 (50 mm x 2 mm) column using 5mM heptafluorbutiric acid/acetonitrile (85:15) as the mobile phase at a flow rate of 0.2 mLmin(-1). The detection of the analyte was achieved by positive ionization electrospray in multiple reaction-monitoring modes. Two characteristic transitions were monitored for streptomycin. Some analytical parameters were validated according to the guidelines laid down by European Commission Decision 2002/657/EC: decision limit, detection capability, recovery, precision and ruggedness. The recoveries of streptomycin from honey fortified at 2.5, 10, 15 and 20 microgkg(-1) levels are around 100%. The decision limit and detection capability of streptomycin was 3 microgkg(-1) and 4.7 microgkg(-1) respectively.

摘要

链霉素是一种氨基糖苷类抗生素,用于养蜂业,保护蜜蜂免受多种幼虫疾病侵害。巴西当局已将其纳入蜂蜜生产国家监管监测计划。已开发并验证了一种使用液相色谱 - 串联质谱法测定蜂蜜中链霉素的简单可靠方法。色谱分离在Gemini 5微米C18(50毫米×2毫米)柱上进行,以5mM七氟丁酸/乙腈(85:15)作为流动相,流速为0.2 mLmin(-1)。通过正离子电喷雾在多反应监测模式下实现对分析物的检测。对链霉素监测了两个特征性跃迁。根据欧盟委员会第2002/657/EC号决定规定的指南,对一些分析参数进行了验证:决策限、检测能力、回收率、精密度和耐用性。在2.5、10、15和20微克/千克水平下添加链霉素的蜂蜜回收率约为100%。链霉素的决策限和检测能力分别为3微克/千克和4.7微克/千克。

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