摘要
建立了动物源性食品和尿液中4种β-受体激动剂克伦特罗、莱克多巴胺、沙丁胺醇和特布他林的超高效液相色谱-串联质谱测定方法。样品均质后，加入乙酸铵水溶液，采用β-葡萄糖醛酸酶／芳基硫酸酯酶酶解处理，过滤后，用Oasis MCX固相萃取柱净化，采用UPLC-MS／MS多反应监测（MRM）模式检测，内标法定量。4种β-受体激动剂的检出限均为0．1μg/kg，定量下限为0．5μg／kg；在0．5、0．75和1.0μg／kg3个浓度添加水平，总体平均回收率为86．7％～114．3％，总体相对标准偏差均在10％以内。本方法分析速度快，灵敏度高，重现性好，各项技术指标均满足国内外相关法规要求，可用于各种动物源性食品及尿液中4种β-受体激动剂残留的快速检测。
A method based on ultra MS/MS） has been developed for the performance liquid chromatography-tandem mass spectrometry （UPLC- determination of beta-agonists residues including clenbuterol, ractopam-ine, salbutamol and terbutalin in products of animal origin and unine. The analytes were extracted with NH4 Ac solution from homogenized samples and hydrolysised with beta-glueuronidase overnight at 37℃. Then the extract was filtered and the filtrate was cleaned by Oasis MCX solid phase extraction cartridge. Quantification of the four analytes was achieved by UPLC-MS/MS with multiple reaction monitoring （MRM） using internal standard method. Detection limits and quantification limits of UPLC-MS/MS for the four analytes were all 0.1 mg/kg and 0.5 mg/kg. The overall recovery varies from 86.7% to 114.3% at the spiked level of 0.5 mg/kg, 0.75 mg/kg, 1.0 mg/kg, and the relative standard deviation （RSD） of the method was less than 10%. The method is reliable, sensitive and reproducible, its performance can meet the requirements of the domestic and international legislation. The method adapts to the determination of beta-agonists residues in different products of animal origin and urine.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2008年第12期1629-1635,共7页
Chinese Journal of Analytical Chemistry
基金
山东出入境检验检疫局科研基金(No.SK200621)资助项目
关键词
β-受体激动剂
动物源性食品
超高效液相色谱-串联质谱
β-Agonists, products of animal origin, ultra performance liquid chromatography- tandem massspectrometry
