同位素稀释-超高效液相色谱-串联质谱法测定鸡蛋中3种类固醇激素  

Quantification of 3 kinds of steroid hormones in eggs by isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry

作　　者：刘宇尘 周剑[1] 王敏[1] 杨梦瑞[1] 王彤彤[1] LIU Yu-Chen;ZHOU Jian;WANG Min;YANG Meng-Rui;WANG Tong-Tong(Institute of Quality Standard and Testing Technology for Agro-products of Chinese Academy of Agricultural Sciences,Key Laboratory of Agri-food Safety and Quality,Beijing 100081,China)

机构地区：[1]中国农业科学院农业质量标准与检测技术研究所,农业农村部农产品质量安全重点实验室,北京100081

出　　处：《食品安全质量检测学报》2021年第24期9334-9341,共8页Journal of Food Safety and Quality

基　　金：国家重点研发计划项目(2019YFC1604802)。

摘　　要：目的建立一种同位素稀释-超高效液相色谱-串联质谱法(isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry, ID-UPLC-MS/MS)检测禽产品中典型类固醇激素(雌酮、孕酮和睾酮)的分析方法。方法样品经乙腈提取,甲醇洗脱后,氮吹至干燥后用1 mL甲醇复溶,上机检测。用0.1%甲酸水溶液(A)和甲醇(B)作流动相进行梯度洗脱,在电喷雾正离子模式和多反应监测模式下采集离子对,检测目标物。结果建立的方法在5min内完成了目标化合物(雌酮、孕酮和睾酮)的定量分析。3种类固醇激素在0.5~100.0μg/kg范围内线性关系良好,r2均大于0.996。雌酮、孕酮和睾酮的方法检出限分别为0.052、0.023和0.048μg/kg,定量限分别为0.173、0.077和0.160μg/kg。在1、5和50μg/kg添加水平下, 3种目标化合物的平均回收率在96.62%~103.11%,精密度在1.36%~3.87%之间。结论该方法简便快速、回收率高、稳定性好,可有效测定禽产品中雌酮、孕酮和睾酮含量。Objective To establish a method for the quantification of 3 kinds of typical steroid hormones(estrone,progesterone and testosterone) in poultry products by isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry(ID-UPLC-MS/MS).Methods The sample was extracted by acetonitrile,eluted by methanol,blown by nitrogen to dry,redissolved with 1 mL methanol,and tested on the machine.Gradient elution was performed with 0.1% formic acid aqueous solution(A) and methanol(B) as mobile phases,ion pairs were collected by electrospray positive ionization mode,and quantitative and qualitative ions were determined by multiple reaction monitoring mode.Results The established method completed the quantitative analysis of target compounds(estrone,progesterone and testosterone) within 5 min.The 3 kinds of steroid hormones had good linear relationships in the range of 0.5-100.0 μg/kg with the correlation coefficients r2 more than 0.996.The limits of detection for estrone,progesterone and testosterone were 0.052,0.023 and 0.048 μg/kg,respectively,and the limits of quantification were 0.173,0.077 and 0.160 μg/kg,respectively.At the addition levels of 1,10 and 50 μg/kg,the average recoveries of the 3 kinds of steroid hormones were 96.62%-103.11%,and the precision was between 1.36% and 3.87%.Conclusion The method is simple,rapid with high recovery rates and good stability,which can effectively determine the content of estrone,progesterone and testosterone in poultry products.

关 键 词：同位素稀释法 超高效液相色谱-串联质谱法 禽产品 类固醇激素 基质效应 

分 类 号：O657.63[理学—分析化学] TS253.7[理学—化学]