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食品研究与开发:2017,38(11):148-152
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UPLC-MS/MS检测运动食品中β-受体激动剂残留
周帅,张飞云
(西安交通大学城市学院,陕西 西安 710018)
Analysis β-Agonist Drugs Residues in Sports Food by UPLC-MS/MS
ZHOU Shuai, ZHANG Fei-yun
(Xi'an Jiaotong University City College, Xi'an 710018, Shaanxi, China)
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投稿时间:2017-02-17    
中文摘要: 建立一种超高效液相色谱-串联质谱法检测运动食品中西马特罗、特步他林、沙丁胺醇、菲诺特罗、莱克多巴 胺、氯丙那林、克伦特罗、妥布特罗、苯乙醇胺 A 和喷布特罗 10 种 β-受体激动剂残留的分析方法。样品前处理用乙腈 沉淀蛋白后,采用 MCX 小柱进行净化和富集。采用 Waters Atalantis T3 色谱柱(2.1 mm×150 mm,3 μm)分离,以 0.1 % 甲酸-乙腈为流动相的梯度洗脱模式下,β-受体激动剂在 1.0 ng/mL~20.0 ng/mL 浓度范围内线性良好,相关系数 r2 为0.993~0.999,检出限为 0.5 μg/kg,定量限为 1.5 μg/kg,加标回收率达到 78.2 %~91.8 %。该方法具有前处理简单、净化 效果好、灵敏度高和检测速度快的优点,适用于运动食品中西马特罗、特步他林、沙丁胺醇、菲诺特罗、莱克多巴胺、氯 丙那林、克伦特罗、妥布特罗、苯乙醇胺 A 和喷布特罗等 10 种 β-受体激动剂残留的分离和定量检测。
Abstract:A ultra high performance liquid chromatography mass spectrometry analysis method was established for the residues determination of cimaterol,terbutaline,salbutamol,fenoterol,rackdopamine,clorprenaline,clen- buterol,tulobuterol,phenylethanolamine A and penbutolol in sports food. After treated with acetonitrile, the sample concentrated and purified by MCX solid phase extraction column. The separation of targeted compound was performed on a Waters Atalantis T3 chromatographic column(2.1 mm×150 mm, 3 μm) using 0.1 % formic acid-acetonitrile as mobile phase under gradient elution mode.The linear range of β-agonist drugs components was in the range of 1.0 ng/mL-20.0 ng/mL with a correlation coefficient of 0.993-0.999. The detection limit was 0.5 μg/kg and the quantitative limit was 1.5 μg/kg.The recovery rate was 78.2 %-91.8 %. The method has the advantages of simple pretreatment, good purifying effect, high sensitivity and fast detection rate, and is suitable for the separation and quantitative detection of cimaterol,terbutaline,salbutamol,fenoterol,rackdopamine,clor- prenaline,clenbuterol,tulobuterol,phenylethanolamine A and penbutolol in sports food.
文章编号:201711033     中图分类号:    文献标志码:A
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