超高效液相色谱-四极杆-飞行时间质谱法测定牛奶中51种激素  

Determination of 51 Hormones in Milk by Ultrahigh Performance Liq⁃uid Chromatography-Quadrupole-Time of Flight Mass Spectrometry

作　　者：段鹤君[1] 张晶[1] 孙佳林 杨润晖 邵兵[1] 牛宇敏[1] DUAN He-jun;ZHANG Jing;SUN Jia-in;YANG Run-hui;SHAO Bing;NIU Yu-min(Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning,Beijing Center for Disease Prevention and Control,Beijing 100013,China;School of Public Health,Capital Medical University,Beijing 100069,China;College of Veterinary Medicine,China Agricultural University,Beijing 100193,China)

机构地区：[1]北京市疾病预防控制中心食物中毒诊断溯源技术北京市重点实验室,北京100013 [2]首都医科大学公共卫生学院,北京100069 [3]中国农业大学兽医学院,北京100193

出　　处：《分析测试学报》2023年第10期1319-1326,共8页Journal of Instrumental Analysis

基　　金：高层次公共卫生技术人才培养计划(学科骨干-01-033)。

摘　　要：基于超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF MS),建立了牛奶中51种激素的高通量筛选和定量方法,并采用信息依赖型采集(IDA)模式建立了51种激素的定性筛选数据库。牛奶样品经乙腈沉淀蛋白后,采用氧化锆包覆硅胶(Z-Sep)填料进一步净化。采用Waters Acquity BEH C_(18)(100 mm×2.1 mm,1.7µm)色谱柱进行分离,UPLC-Q-TOF MS测定,基质匹配曲线外标法定量。牛奶中51种激素的线性范围为0.10~500µg/L,相关系数(r^(2))均大于0.99;检出限为0.03~1.67µg/kg,定量下限为0.10~5.00µg/kg;在5、10、50µg/kg加标水平下的回收率为44.6%~120%,相对标准偏差为0.90%~20%。利用该方法测定了20份市售牛奶样品,其中19份样品检出孕酮,检出量为0.80~4.51µg/kg;1份样品中含有痕量的氢化可的松,检出量为0.62µg/kg;其他激素均未检出。该方法具有良好的线性、灵敏度、准确度和精密度,可用于多种激素的同时定性定量分析。A comprehensive high-throughput screening and quantification method for hormones was established based on ultrahigh performance liquid chromatography-quadrupole-time of flight mass spectrometry(UPLC-Q-TOF MS).A database for qualitative screening of 51 hormones was estab-lished using information dependent acquisition(IDA)mode.After precipitation of protein in milk samples by acetonitrile,the milk samples were purified using zirconia coated silica gel sorbent(Z-Sep).Separation was performed on Waters Acquity BEH C_(18) column(100 mm×2.1 mm,1.7µm)with gradient elution by UPLC-Q-TOF MS and quantified using matrix matching curve external stan-dard method.The method showed good linearity in the range of 0.10-500µg/L,with correlation co-efficients(r^(2))greater than 0.99.The limits of detection(LODs)and limits of quantitation(LOQs)were in the range of 0.03-1.67µg/kg and 0.10-5.00µg/kg,respectively.The recoveries is 44.6%-120%with relative standard deviations of 0.90%-20%.Twenty milk samples were determined using this method,of which 19 samples were detected for progesterone,with content ranged from 0.80 to 4.51µg/kg,one sample had trace amounts of cortisol detected at 0.62µg/kg,and no other hormones were detected.This method has good linearity,sensitivity,accuracy,and precision,and can beused for simultaneous qualitative and quantitative analysis of multiple hormones.

关 键 词：激素 牛奶 超高效液相色谱-四极杆-飞行时间质谱 QUECHERS 

分 类 号：O657.63[理学—分析化学] TS201.6[理学—化学]