摘要
目的建立新型固相萃取技术结合超高效液相色谱串联质谱测定猪肉中17种β-受体阻断剂的测定方法。方法猪肉样品经酶解,乙腈沉淀蛋白并萃取后,经Oasis PRiME HLB固相萃取柱通过式净化。以甲醇和0.1%甲酸水为流动相梯度洗脱,采用迪马Endeavorsil C18色谱柱分离,ESI源正离子模式进行多反应监测(MRM),内标法定量。结果17种β-受体阻断剂的线性范围在0.2~20μg/L,相关系数(r)>0.999,检出限(LOD)为0.05~0.07μg/kg,定量限(LOQ)为0.15~0.2μg/kg。3个加标水平下(0.2、0.4、2μg/kg)的回收率为84.97%~123.40%,RSD为0.41%~13.94%。结论本方法灵敏、快速、准确,可用于猪肉中β-受体阻断剂的定性、定量检测。
Objective A sensitive and rapid method was developed for the determination of 17β-adrenergic receptor blockers(β-blockers)by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS).Methods Theβ-blockers were extracted from porcine sample with acetonitrile,purified by solid phase extraction column Oasis Prime HLB.The analytes were then separated by the Endeavorsil C18 chromarographic column with methanol and 0.1%formic acid as gradient mobile phase.The ion fragment information analytes were obtained using ultra performance liquid chromatography-tandem mass spectrometry under multiple reaction monitoring mode and the isotope internal standards were used to quantify by calibration curves.Results The linear ranges of 17β-blockers were from 0.2 to 20μg/kg,with correlation coefficient(R)>0.999.The limits of detection(LOD)were 0.05-0.07μg/kg,and the limits of quantification(LOQ)were 0.15-0.2μg/kg.The average recoveries ofβ-blockers(added into blank porcine samples at three concentration levels)ranged from 84.97%to 123.40%,and the relative standard deviation(RSD)was 0.41%to 13.94%.Conclusion The method is simple,sensitive,accurate and is suitable for the confirmation and quantification ofβ-blockers in porcine samples.
作者
屠瑞莹
范赛
张楠
赵海燕
李兵
吴国华
赵榕
TU Ruiying;FAN Sai;ZHANG Nan;ZHAO Haiyan;LI Bing;WU Guohua;ZHAO Rong(Beijing Center for Preventive Medicine Research,Beijing 100013,China;Beijing Center for Disease Prevention and Control,Beijing 100013,China)
出处
《中国食品卫生杂志》
CSCD
北大核心
2021年第5期571-577,共7页
Chinese Journal of Food Hygiene
关键词
超高效液相色谱串联质谱
Β-受体阻断剂
猪肉
固相萃取
Ultra performance liquid chromatography tandem mass spectrometry
β-blockers
porcine
solid phase extraction
