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使用液相色谱-串联质谱法对牛尿液中玉米赤霉醇、他莫昔芬和镰刀菌属毒素进行确证分析。

Confirmatory assay for zeranol, taleranol and the Fusarium spp. toxins in bovine urine using liquid chromatography-tandem mass spectrometry.

作者信息

Launay F M, Young P B, Sterk S S, Blokland M H, Kennedy D G

机构信息

Queen's University Belfast, Department of Veterinary Science, UK.

出版信息

Food Addit Contam. 2004 Jan;21(1):52-62. doi: 10.1080/02652030310001636930.

Abstract

A method is described for the quantitative determination of the veterinary drug zeranol, its epimer taleranol and the mycotoxins zearalenone, alpha-zearalenol and beta-zearalenol in bovine urine. The method is based on liquid chromatography coupled to negative-ion electrospray mass spectrometry-mass spectrometry of urine extracts prepared by solid-phase extraction with C(18) columns. Two transition ions at m/z 277 and 91 are monitored for zeranol and taleranol along with the transition ion at m/z 281 for their respective deuterated (d(4)) internal standards. Similarly, two transitions are monitored for each of the three mycotoxins along with a transition ion for each of their corresponding internal standards. The method has been validated according to the new European Union criteria for analysis of veterinary drug residues, and is suitable for monitoring urine samples taken under National Surveillance Schemes. The method has been validated at 1, 1.5 and 2 ng ml(-1) for zeranol and taleranol and at 5, 10 and 15 ng ml(-1) for each of the three mycotoxins. Correlation between the described method and a routine method, based on gas chromatography-mass spectrometry, was assessed using a range of naturally incurred samples.

摘要

本文描述了一种用于定量测定牛尿液中兽药玉米赤霉醇、其差向异构体taleranol以及霉菌毒素玉米赤霉烯酮、α-玉米赤霉醇和β-玉米赤霉醇的方法。该方法基于液相色谱与负离子电喷雾质谱联用,对用C(18)柱固相萃取制备的尿液提取物进行质谱分析。监测玉米赤霉醇和taleranol的质荷比为277和91的两个跃迁离子,以及它们各自的氘代(d(4))内标的质荷比为281的跃迁离子。同样,对三种霉菌毒素中的每一种监测两个跃迁,以及它们各自相应内标的一个跃迁离子。该方法已根据欧盟兽药残留分析的新标准进行了验证,适用于监测国家监测计划下采集的尿液样本。该方法对玉米赤霉醇和taleranol在1、1.5和2 ng ml(-1)浓度下进行了验证,对三种霉菌毒素中的每一种在5、10和15 ng ml(-1)浓度下进行了验证。使用一系列自然污染的样本评估了所述方法与基于气相色谱-质谱联用的常规方法之间的相关性。

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