Analysis of 13 kinds of steroid hormones in raw milk using modified QuEChERS method combined with UPLC-QTOF-MS

作     者：TAN Xin-tong LI Zeng-mei DENG Li-gang ZHAO Shan-cang WANG Ming-lin 

作者机构：Academy of Food Science and Engineering Shandong Agricultural University Tai'an 271018 P.R. China Institute of Agricultural Quality Standards and Testing Technology Research Shandong Academy of Agricultural Sciences Jinan 250100 P.R.China Key Laboratory of Test Technology on Food Quality and Safety of Shandong Province Jinan 250100 P.R. China 

出 版 物：《Journal of Integrative Agriculture》 (农业科学学报（英文版）)

年 卷 期：2016年第15卷第9期

页      面：2163-2174页

核心收录：

学科分类：0832[工学-食品科学与工程（可授工学、农学学位）] 08[工学] 083203[工学-农产品加工及贮藏工程] 

基　　金：supported by the Natural Science Foundation of Shandong Province,China(ZR2015CM015) the Special Fund for Agro-Scientific Research in the Public Interest,China(201403071) 

主　　题：UPLC QTOF MS raw milk QuEChERS steroid hormones acidic alumina 

摘      要：Thirteen kinds of steroid hormones in raw milk（cow, goat and buffalo milk） were analyzed with ultra performance liquid chromatography-quadrupole time of flight mass spectrometry（UPLC-QTOF-MS） after extraction and cleanup with the modified Qu ECh ERS method. These steroid hormones included 17β-estradiol, estriol, estrone, diethylstilbestrol, progesterone, melengestrol acetate, megestrol acetate, chlormadinone acetate, 19-nortestosterone, metandienone, boldenone, epitestosterone, and testosterone. The limits of detection for the raw milk basing on 3 times the signal to noise ratios（S/N=3） was in range of 0.07-0.51 μg kg^–1, and the limits of quantification（basing on S/N=10 method） covered the ranges from 0.23 to 1.7 μg kg^–1. With matrix external standard method, the substances presented recoveries over the range 74.2–99.7%. Qualitative analysis was also done in the mass/mass spectrum（MS/MS） mode and each debris structure of 13 kinds of steroid hormones was achieved. The methodology was then applied in real raw milk samples which were collected in several areas of China and the progesterone was detected with high level.