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液相色谱-串联质谱法测定肝脏和视网膜中的β-激动剂。

Determination of beta-agonists in liver and retina by liquid chromatography-tandem mass spectrometry.

作者信息

Fesser Adrian C E, Dickson Leslie C, MacNeil James D, Patterson John R, Lee Stephen, Gedir Ronald

机构信息

Centre for Veterinary Drug Residues, Canadian Food Inspection Agency, Saskatoon Laboratory, 116 Veterinary Rd, Saskatoon, S7N 2R3, Canada.

出版信息

J AOAC Int. 2005 Jan-Feb;88(1):61-9.

Abstract

A liquid chromatography-tandem mass spectrometry (LC/MS/MS) method for the determination of bromobuterol, cimaterol, clenbuterol, clenpenterol, hydroxymethylclenbuterol, isoxsuprine, mabuterol, ractopamine, ritrodrine, salbutamol, terbutaline, and tulobuterol residues in bovine liver and retina is reported. This procedure uses enzymatic digestion, liquid-liquid extraction, and cleanup on Oasis HLB solid-phase extraction cartridges, followed by determination of the residues by LC-tandem quadrupole MS using atmospheric pressure chemical ionization in the positive ion mode. Overall average recoveries ranged from 23 to 76% for liver and 34 to 77% for retina. The mean values for samples fortified at levels between 0.5-2.0 microg/kg (liver) and 5-20 microg/kg (retina) agreed within 98-118% of the spiked levels, with coefficients of variation ranging from 6 to 20%. The decision limits, CCalpha, ranged from 0.1 to 0.3 microg/kg for liver, 1-3 microg/kg for retina, and detection capabilities, CCbeta, from 0.2-0.5 microg/kg for liver and 2-5 microg/kg for retina.

摘要

报道了一种液相色谱-串联质谱(LC/MS/MS)法,用于测定牛肝和视网膜中溴布特罗、西马特罗、克伦特罗、氯丙那林、羟甲基克伦特罗、异克舒令、马布特罗、莱克多巴胺、利托君、沙丁胺醇、特布他林和妥布特罗的残留量。该方法采用酶解、液液萃取,并在Oasis HLB固相萃取柱上进行净化,然后通过液相色谱-串联四极杆质谱,在正离子模式下采用大气压化学电离测定残留量。肝脏的总体平均回收率为23%至76%,视网膜的总体平均回收率为34%至77%。在0.5 - 2.0微克/千克(肝脏)和5 - 20微克/千克(视网膜)加标水平下的样品平均值在加标水平的98%至118%范围内,变异系数为6%至20%。肝脏的决策限CCalpha为0.1至0.3微克/千克,视网膜为1 - 3微克/千克,肝脏的检测能力CCbeta为0.2 - 0.5微克/千克,视网膜为2 - 5微克/千克。

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