Journal of Integrative Agriculture ›› 2016, Vol. 15 ›› Issue (9): 2163-2174.DOI: 10.1016/S2095-3119(16)61386-2

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  • 收稿日期:2015-11-04 出版日期:2016-09-02 发布日期:2016-09-02

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

AN Xin-tong1, LI Zeng-mei2, 3, DENG Li-gang2, 3, ZHAO Shan-cang2, 3, WANG Ming-lin1   

  1. 1 Academy of Food Science and Engineering, Shandong Agricultural University, Tai’an 271018, P.R.China
    2 Institute of Agricultural Quality Standards and Testing Technology Research, Shandong Academy of Agricultural Sciences, Jinan 250100, P.R.China
    3 Key Laboratory of Test Technology on Food Quality and Safety of Shandong Province, Jinan 250100, P.R.China
  • Received:2015-11-04 Online:2016-09-02 Published:2016-09-02
  • Contact: WANG Ming-lin, Tel: +86-538-8246029, Fax: +86-538-8249157, E-mail: mlwang1963@163.com
  • About author:TAN Xin-tong, E-mail: tanxintong142536@163.com;
  • Supported by:

    This research was supported by the Natural Science Foundation of Shandong Province, China (ZR2015CM015) and the Special Fund for Agro-Scientific Research in the Public Interest, China (201403071). The authors show great appreciation to Shandong Academy of Agricultural Sciences, China, for supporting the laboratory equipments.

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Abstract:     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 QuEChERS 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.

Key words: UPLC-QTOF-MS ,  raw milk ,  QuEChERS ,  steroid hormones ,  acidic alumina