液相色谱-串联质谱法测定动物肌肉和牛奶中的雌二醇  

Determination of estradiol in animal muscle and milk by liquid chromatography-tandem mass spectrometry

作　　者：杨奕[1] 杨蕴嘉[1] 尹杰[1] 张晶[1] YANG Yi;YANG Yun-Jia;YIN Jie;ZHANG Jing(Bejing Center for Disease Prevention and Control,Beijing Research Center for Preventive Medicine,Beijing 100013,China)

机构地区：[1]北京市疾病预防控制中心,北京市预防医学研究中心,北京100013

出　　处：《食品安全质量检测学报》2021年第9期3652-3657,共6页Journal of Food Safety and Quality

基　　金：国家重点研发计划(2017YFC1601600)。

摘　　要：目的建立丹磺酰氯衍生液相色谱-串联四极杆质谱法检测鸡肉、牛肉、牛奶中雌二醇的高灵敏分析方法。方法酶解后的样品用HLB和氨基固相萃取柱富集净化,氮气吹干后,在60℃条件下丹磺酰氯衍生5 min;以乙腈-水(含0.1%乙酸)为流动相,采用多离子反应监测正离子模式进行检测。结果鸡肉、牛肉、牛奶中雌二醇的检出限为0.6 ng/kg,定量限为2.0 ng/kg,3个添加水平的平均回收率在82.0%~88.9%之间,相对标准偏差均小于7.3%。我国6个城市牛肉、鸡肉和牛奶中17-β-雌二醇含量的中位数(平均值)分别为5.51 ng/kg(66.78 ng/kg)、4.60 ng/kg(16.94 ng/kg)和18.00 ng/kg(16.80 ng/kg),九十百分位数(P90)分别为248.91、39.33和39.60 ng/kg。结论本方法适用动物肌肉和乳中超痕量雌二醇的含量检测。牛肉、鸡肉和牛奶中17-β-雌二醇的大样本监测数据可为科学的制定残留限量提供必要的数据基础。Objective To establish a highly sensitive analytical method for the determination of estradiol in chicken,beef and milk by dansyl chloride derivative liquid chromatography-tandem quadrupole mass spectrometry.Methods The samples after enzymolysis were enriched and purified by HLB and amino solid-phase extraction columns,dried by nitrogen,and derivatized with dansyl chloride at 60℃for 5 min.Acetonitrile-water(containing 0.1%acetic acid)was used as the mobile phase,and the detection was conducted in a positive ion mode using multi-ion reaction monitoring.Results The detection limit and quantitation limit of estradiol in chicken,beef,and milk were 0.6 ng/kg and 2.0 ng/kg,respectively.The average recoveries of the 3 spiked levels were within the range of 82.0%-88.9%,and the relative standard deviations were all less than 7.3%.The median(mean)values of 17-β-estradiol in beef,chicken,and milk from six cities in China were 5.51 ng/kg(66.78 ng/kg),4.60 ng/kg(16.94 ng/kg)and 18.00 ng/kg(16.80 ng/kg),respectively,and the ninetieth percentile(P90)values were 248.91,39.33,and 39.60 ng/kg,respectively.Conclusion This method is suitable for the determination of ultra-trace estradiol in muscle and milk of animals.The large sample monitoring data of 17-β-estradiol in beef,chicken and milk can provide the necessary data basis for the scientific formulation of residue limits.

关 键 词：雌二醇 液相色谱-串联质谱法 丹磺酰氯 衍生 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学] TS252.7[轻工技术与工程—农产品加工及贮藏工程]