超高效液相色谱三重四极杆质谱法同时快速测定动物源食品中6种β受体兴奋剂残留  

Rapid simultaneous determination of six β-agonists in foodstuffs of animal origin by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry

作　　者：蔡欣欣[1] 张秀尧[1] 

机构地区：[1]浙江省温州市疾病预防控制中心,浙江温州325001

出　　处：《中国卫生检验杂志》2008年第7期1252-1255,共4页Chinese Journal of Health Laboratory Technology

基　　金：温州市医药卫生科研课题(2006B079)

摘　　要：目的：建立简单、快速、同时测定动物源食品中6种β受体兴奋剂残留的超高效液相色谱三重四极杆质谱确证检测方法。方法：1．00g样品用10ml含0．1％乙酸的乙腈液一次提取、经5g无水硫酸钠和10ml正己烷同时脱水脱脂后，5．0ml乙腈提取液氮气吹干，残渣溶于1．0ml 10％甲醇水液，再经2ml正己烷萃取脱脂，UPLC HSS T3柱超高效液相色谱分离后电喷雾串联质谱法检测，采用正离子方式多反应监测，基体标准定量。结果：加标水平为1．0、5．0和10．0μg/kg时，盐酸克伦特罗、沙丁胺醇、特布他林和妥洛特罗的回收率在79．4％～124．5％之间，相对标准偏差为1．2％-13．5％（n=5），莱克多巴胺和丙卡特罗回收率在59．2％～124．5％范围内，相对标准偏差为3．7％～20％（n=5）。方法的定量限和确证限分别在0．02～1．0μg/kg和0．10～1．0μg/kg之间。结论：本法快速、准确，操作简单，两位检测人员可在3h内处理20份已绞碎均质的样品，特别适合大批量样品的快速分析。Objective： A new approach for simple and rapid simultaneous determination of six β - agonists in foodstuffs of animal origin by ultra - performance liquid chromatography - tandem mass spectrometry is desciibed. Methods： The procedure involves a single extraction of 1.00 g of sample with 10 ml of acetonitrile containing 0. 1% acetic acid, followed by liquid-liquid partitioning formed by addition of 10 ml of n - hexane plus 5 g of anhydrous Na2SO4. The 5.0 ml of acetonitrile extract was transferred and evaporated to dryness under nitrogen stream at 50℃. The residue was reconstituted in 1.0 ml of 10% methanol Lipids in the extracts were removed by liquid -liquid partiton with n -hexane again. The Analytes were separated by UPLC with an UP- LC HSS T3 column under gradient of 0. 1% formate acid and 0. 1% formate acid in methanol, and detected using a positive electrospray ionization tandem mass spectrometry in the MRM mode, and quantified by matrix - match standard solution. Results： The standard curve was linear over the concentration range of 0. 5 - 20 ng/mL The average recoveries for clenbuterol hydrochloride, salbutamol, terbutalin and tulobuterol ranged from 79. 4% to 124. 5% with the relative standard deviation 1.2% - 13. 5% （n = 5） and that for ractopamine and procaterol were from 59. 2% to 124. 5% with the RSD 3.7% -20% （n =5）. Estimated values for the limit of quantification （ LOQ ） and the limit of confirmation （LOC） for six β - agonists were whithin 0. 02 - L 0 μg/kg and 0. 10 - 1.0μg/kg , respectively. Conclusion：Using this method, two chemists can prepare a batch of 20 previously homogenised samples within 3 hours. This method should be useful in supporting regulatory enforcement programs that monitor β - agonist misuse.

关 键 词：Β受体兴奋剂 多残留分析 超高效液相色谱三重四极杆质谱法 动物源食品 克伦特罗 沙丁胺醇 特布他林 莱克多巴胺 丙卡特罗 妥洛特罗 

分 类 号：O657.63[理学—分析化学]