HPLC-MS/MS Determination of Residual Amounts of 4 β-Agonists in Foodstuffs of Animal Origin
摘 要
采用高效液相色谱-串联质谱法同时测定动物源性食品中4种β-兴奋剂克伦特罗、莱克多巴胺、沙丁胺醇、特布他林的残留量.样品用乙酸铵缓冲溶液提取,过LC-18 Sep Pak和LC-SCX Sep Pak固相萃取柱净化,将淋出液蒸发浓缩后用乙腈-水(10+90)定容.通过C18色谱柱分离,流出液供串联质谱测定,同位素内标法定量.4种β-兴奋剂克伦特罗、沙丁胺醇、莱克多巴胺、特布他林的质量浓度与其峰面积均呈线性关系,检出限(3S/N)分别为0.05,0.1,0.1,0.1 μg·kg-1.猪肝中克伦特罗、莱克多巴胺、沙丁胺醇、特布他林的回收率分别为91.8%~99.0%,98.3%~105.5%,76.8%~82.8%,75.1%~85.2%,相对标准偏差(n=7)均小于12.5%.
Abstract
High performance liquid chromatography in hyphenation with tandem mass spectrometry (HPLC-MS/MS) was applied to the determination of residual amounts of 4 kinds of β-agonists,including celenbuterol,salbutamol,raotopamine and terbutalin in foodstuffs.The sample was extracted with ammonium acetate buffer solution,which was concentrated and purified by LC-18 Sep Pak and LC-SCX Sep Pak solid-phase extraction column.The eluate was evaporated to near dryness and diluted to a definite volume with acetonitrile-H2O(10+90) solution,and separated on the C18 column.The eluate was used for tandem MS analysis.External standard calibration of isotope was adopted in the determination.Linear relationships between values of peak area and mass concentration of celenbuterol,raotopamine,salbutamol and terbutalin were obtained,with their detection limits of 0.05,0.1,0.1,0.1 μg·kg-1 respectively.Values of recovery of celenbuterol,salbutamol,raotopamine and terbutalin in the range of 91.8%-99.0%,98.3%-105.5%,76.8%-82.8% and 75.1%-85.2% were found respectively in a sample pig liver.Values of RSD′s (n=7) found were less than 12.5%.
中图分类号 O657.63
所属栏目 工作简报
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收稿日期 2008/4/16
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备注赵善贞(1983-),女,上海市人,硕士研究生,从事食品科学研究.
引用该论文: ZHAO Shan-zhen,CHEN Shun-sheng,DENG Xiao-jun,YIN Ping. HPLC-MS/MS Determination of Residual Amounts of 4 β-Agonists in Foodstuffs of Animal Origin[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(8): 968~971
赵善贞,陈舜胜,邓晓军,殷平. 高效液相色谱-串联质谱法测定动物源性食品的4种β-兴奋剂残留量[J]. 理化检验-化学分册, 2009, 45(8): 968~971
被引情况:
【1】李莺,李婵君,王楠, "气相色谱-质谱法测定猪肉中盐酸克伦特罗残留量",理化检验-化学分册 50, 1149-1152(2014)
【2】张静,张静, "涂丝型聚氯乙烯膜-硫酸沙丁胺醇电极的研制与应用",理化检验-化学分册 50, 1220-1222(2014)
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参考文献
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【2】杨艳艳,王选年,魏红,等.猪尿液中盐酸克伦特罗残留的ELISA法和GC-MS法检测[J].中国兽医杂志,2004,40(1):9-11.
【3】金雁,姚家彪,姜莉,等.高效液相色谱法同时测定禽肉中的克伦特罗和沙丁胺醇[J].现代仪器,2005,15:34-37.
【4】刘军,刘清,李志强,等.高效液相色谱法测定肉类中克伦特罗等激素类生长促进剂残留量[J].理化检验-化学分册,2005,41(7):504-506.
【5】谢孟峡,刘媛.固相萃取-气相色谱/质谱分析肉样中盐酸克伦特罗的残留量[J].分析化学,2002,30(11):1308-1311.
【6】朱坚,李波,方晓明等.气相色谱-质谱法测定肝、肾和肉中11种β-受体激动剂残留量[J].质谱学报,2005,26(3):129-137.
【7】JOSE B,MUNOZ P,MORGADO M,et al.Determin of clenbuterol,ractopamine and zilpaterol in liver and urine by liquid chromatography tandem mass spectometry[J].Anal Chim Acta,2005,529:199-205.
【8】JOSEPH H W,LAU C S,JOHN E M.Determination of clenbuterol,salbutamol,and cimaterol in bovine retina by electrospray ionization-liquid chromatography-tandem mass spectrometry[J].Journal of AOAC International,2004,87(1):31-38.
【9】刘红霞,张书胜,张西林,等.猪肝脏和肌肉组织中β-兴奋剂克伦特罗的高效液相色谱电喷雾质谱分析研究[J].分析化学,2004,32:801-804.
【10】吉彩霓,岳振峰,欧阳姗.固相萃取-高效液相色谱/串联质谱法同时测定猪肉中克伦特罗和沙丁胺醇残留[J].中华预防医学杂志,2006,40(2):123-125.
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