摘要
建立在线固相萃取-高效液相色谱-串联质谱检测猪肉及羊肉中10种β-受体激动剂的全自动分析方法。样品于37℃酶解16 h后,经MCX在线固相萃取小柱净化,采用XBridge C_(18)色谱柱分离,以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,在电喷雾电离正离子模式下,采用多反应监测模式检测,内标法定量。结果表明:10种β-受体激动剂在0.01～10.00 ng/mL范围内线性关系良好,相关系数均大于0.999 0;检出限为0.004～0.040μg/kg,定量限为0.02～0.20μg/kg;方法回收率为76.5%～107.7%,相对标准偏差小于10%。该方法分析速度快、灵敏度高,可用于猪肉和羊肉中10种β-受体激动剂的定性及定量分析。
In this research, we developed a fully automated method to determine 10 β-agonists in pork and lamb using on-line solid phase extraction coupled to high performance liquid chromatography-tandem mass spectrometry（HPLC-MS-MS）. After being enzymatically digested at 37 ℃ for 16 h, samples were purified by on-line solid phase extraction on an MCX column, and then separated on an XBridge C18 column by gradient elution using 0.1% formic acid solution and acetonitrile as the mobile phase. Mass spectrometric data were acquired under multiple reaction monitoring（MRM） mode using positive ion electrospray ionization. Quantitation was performed by the internal standard method. The results showed a good linear relationship in the concentration range of 0.01–10.00 ng/m L was achieved for all analytes with acorrelation coefficient higher than 0.999 0. The limits of detection（LOD） were in the range of 0.004–0.040 μg/kg and the limits of quantitation（LOQ） were in the range of 0.02–0.20 μg/kg. The recoveries of the method ranged from 76.5% to 107.7%, with relative standard deviation（RSD）lower than 10%. These results demonstrate that the method is simple, sensitive, and can be used for quantification of 10 β-agonists in pork and lamb samples.
作者
马俊美
孙磊
刘茁
沈璐
张冬生
贾文轩
李强
范素芳
MA Junmei;SUN Lei;LIU Zhuo;SHEN Lu;ZHANG Dongsheng;JIA Wenxuan;LI Qiang;FAN Sufang(Hebei Food Inspection and Research Institute,Shijiazhuang 050000,China;College of Bioscience and Bioengineering,Hebei University of Science and Technology,Shijiazhuang 050018,China)
出处
《肉类研究》
北大核心
2018年第5期19-25,共7页
Meat Research
基金
河北省食品药品监督管理局科技计划项目(QN2015001)
国家重大科学仪器设备开发专项(2012YQ0301110602)
关键词
在线固相萃取
高效液相色谱-串联质谱法
β-受体激动剂
内标法定量
on-line solid phase extraction
liquid chromatography-tandem mass spectrometry
β-agonists
internal standard method
