摘要
目的:建立了采用超高效液相色谱-四极杆/飞行时间质谱法对液态奶中的氟他胺和羟基氟他胺进行测定的方法。方法:样品用水稀释,乙酸乙酯提取后,盐析分层,经十八烷基键合硅胶(C_(18))固相萃取剂净化后,氮气浓缩至近干,乙腈复溶,采用ESI源负离子扫描方式进行分析。结果:氟他胺和羟基氟他胺的基质曲线在1.0~100.0μg·L^(-1)线性关系良好,相关系数R^(2)大于0.999,平均回收率为94.8%~108.0%,RSD为1.58%~5.58%。方法检出限均为2.0μg·kg^(-1),方法定量限均为5.0μg·kg^(-1)。结论:该方法定性定量能力强,回收率好、灵敏度高和重现性好,可用于日常的筛查及测定。
Objective: An ultra performance liquid chromatography-quadrupole/time-of-flight mass spectrometry determination method was established for flutamide and hydroxyflutamide in liquid milk. Method: The sample is diluted with water, extracted with ethyl acetate, salted out and layered, purified by octadecyl bonded silica gel(C_(18)) solid phase extractant, concentrated to nearly dry with nitrogen, redissolved with acetonitrile, and analyzed by ESI source anion scanning.Result: The matrix curve of flutamide and hydroxyflutamide showed a good linear relationship ranged from 1.0 μg·L^(-1) to 100.0 μg·L^(-1) with the correlation coefficient R^(2) was greater than 0.999. The average recovery was 94.8%~108.0%, RSD was 1.58%~5.58%. The limits of detection were both 2.0 μg·kg^(-1) and the limits of quantification were 5.0 μg·kg^(-1). Conclusion:This method has strong qualitative and quantitative ability, good recovery, high sensitivity and reproducibility, and can be used for daily screening and determination.
作者
李文倩
李俞洁
曾令浩
吴图政
李思萦
章海涛
LI Wenqian;LI Yujie;ZENG Linghao;WU Tuzheng;LI Siying;ZHANG Haitao(Guangzhou Inspection and Testing Certification Group Co.,Ltd.,National Quality Testing Center for Processed Food(Guangdong),Guangzhou 511447,China;Zhanjiang Institute of Supervision&Test on Quality&Measure,Zhanjiang 524000,China;Guangzhou Customs Technology Center,Guangzhou 510623,China)
出处
《现代食品》
2022年第18期176-180,共5页
Modern Food
关键词
超高效液相色谱-四极杆/飞行时间质谱
分散固相萃取
液态奶
氟他胺
羟基氟他胺
ultra performance liquid chromatography-quadrupole/time-of-flight mass spectrometry
dispersive solid phase extraction
liquid milk
flutamide
hydroxyflutamide
