新型净化材料结合QuEChERS技术用于动物肌肉组织中β-受体激动剂的快速检测  

Rapid determination of β-agonists in meat by QuEChERS technology with a new purification material

作　　者：张景然 张建柱[2] 杨影 ZHANG Jing-Ran;ZHANG Jian-Zhu;YANG Ying(College of Food Engineering and Biotechnology, Tianjin University of Science and Technology, Tianjin 300457, China;Tianjin Bona Agela Technologies Co., Ltd., Tianjin 300462, China)

机构地区：[1]天津科技大学食品工程与生物技术学院,天津300457 [2]天津博纳艾杰尔科技有限公司,天津300462

出　　处：《食品安全质量检测学报》2019年第10期3097-3105,共9页Journal of Food Safety and Quality

摘　　要：目的建立食用肉类中9种β-受体激动剂残留的QuEChERS-液相色谱-三重四极杆质谱(liquid chromatography-tandem mass spectrometry, LC-MS/MS)的检测方法。方法样品经酶解后,用1%氨化乙腈提取,无水硫酸镁盐析后取乙腈相,经新型净化材料分散固相萃取法净化。采用Kinetex 2.6μm F5(3.0 mm×50 mm,2.6μm)色谱柱,经0.1%甲酸水溶液(A)和0.1%甲酸乙腈溶液(B)梯度洗脱,于电喷雾正离子源(electrospray ionization, ESI+)和多反应监测模式(multiple reaction monitoring, MRM)下监测,基质标准曲线定量。结果9种β-受体激动剂在不同添加水平下,相对回收率为70.2%~100.0%, RSD在1.0%~14.9%(n=3),检出限为0.002~0.190μg/kg,定量限为0.01~0.76μg/kg。结论该方法操作简便、快速、净化效果好、准确性高,适用于食用肉类中β-受体激动剂的残留确证。Objective To establish a method for determination of 9 kinds of β-agonists residues in meat by QuEChERS-liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Meat samples were extracted with 1% ammonia acetonitrile after enzymolysis, salted out by MgSO4, and then the organic phase were cleaned up by a new purification QuEChERS material. A Kinetex- 2.6μm F5 (3.0 mm×50 mm, 2.6 μm) column was used for separation, with a gradient elution program of 0.1% formic acid aqueous solution (A) and 0.1% formic acid in acetonitrile solution (B). ESI positive ion scan was used under multiple reaction monitoring (MRM) mode and quantified by matrix-matched external standard method. Results At different additional levels, the recoveries of 9 kinds of agonists were in the range of 70.2%-100.0% with the relative standard deviations of 1.0%-14.9%(n=3). The limits of detections were 0.002-0.190 μg/kg and the limits of quantitative were 0.01-0.76 μg/kg. Conclusion The method is simple, fast, accurate and has prominent effect in degreasing, which is suitable for detecting the agonists residues in meat.

关 键 词：QUECHERS 液相色谱-串联质谱法 β-受体激动剂 新型净化材料 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学]