超高效液相色谱-四极杆飞行时间质谱法测定液态奶中的氟他胺和羟基氟他胺  

Determination of Flutamide and Hydroxyflutamide in Liquid Milk by Ultra Performance Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometry

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)

机构地区：[1]广州检验检测认证集团有限公司,国家加工食品质量检验中心,广东广州511447 [2]广东省湛江市质量计量监督检测所,广东湛江524000 [3]广州海关技术中心,广东广州510623

出　　处：《现代食品》2022年第18期176-180,共5页Modern Food

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.

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 

分 类 号：O657.63[理学—分析化学]