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育肥牛中作为饲料添加剂的齐帕特罗的提取、净化及气相色谱-质谱表征

Extraction, clean-up and gas chromatography-mass spectrometry characterization of zilpaterol as feed additive in fattening cattle.

作者信息

Bocca B, Di Mattia M, Cartoni C, Fiori M, Felli M, Neri B, Brambilla G

机构信息

Istituto Superiore di Sanità, Laboratorio Medicina Veterinaria, Viale Regina Elena 299, 00161, Rome, Italy.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2003 Jan 5;783(1):141-9. doi: 10.1016/s1570-0232(02)00528-7.

Abstract

Zilpaterol is an adrenergic drug currently licensed in Mexico and South Africa as a feed additive for cattle close to consignment. In this study an analytical method to detect zilpaterol in commercial feeds was set up. The influence of extraction solvent and matrix was evaluated. The drug as a trimethylsilyl derivative was characterized by GC-MS, on a quadrupole detector, in the electron impact mode. Acidic extraction, solid-phase extraction C(18) non-endcapped clean-up and mass characterization on ions m/z 308, 291, 405, 390 provided zilpaterol recoveries >75.3% and repeatability <3.3% in feeds spiked in the range 30.0-120.0 ng/g. The limits of detection and quantification were 7.5 and 25.0 ng/g, respectively. Such limits are well below the dose of 5.0-20.0 microgram/g proposed as effective.

摘要

齐帕特罗是一种肾上腺素能药物,目前在墨西哥和南非被许可用作待托运牛的饲料添加剂。在本研究中,建立了一种检测商业饲料中齐帕特罗的分析方法。评估了萃取溶剂和基质的影响。该药物作为三甲基硅烷基衍生物,通过气相色谱 - 质谱联用仪在四极杆检测器上以电子轰击模式进行表征。酸性萃取、固相萃取C(18)非封端净化以及对离子m/z 308、291、405、390的质谱表征,使得在添加量为30.0 - 120.0 ng/g的饲料中齐帕特罗的回收率>75.3%,重复性<3.3%。检测限和定量限分别为7.5和25.0 ng/g。这些限值远低于提议的有效剂量5.0 - 20.0微克/克。

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