YU Hui-juan, ZHANG Shan-shan, ZHANG Xiao-ling, HUI Yun-hua, GU Run-run, FENG Bing. Simultaneous Determination of the Estrogen, Progestogen and Androgen in Aquatic Products by Isotope Dilution LC-MS/MS[J]. Journal of Chinese Mass Spectrometry Society, 2014, 35(2): 170-178. DOI: 10.7538/zpxb.2014.35.02.0170
Citation: YU Hui-juan, ZHANG Shan-shan, ZHANG Xiao-ling, HUI Yun-hua, GU Run-run, FENG Bing. Simultaneous Determination of the Estrogen, Progestogen and Androgen in Aquatic Products by Isotope Dilution LC-MS/MS[J]. Journal of Chinese Mass Spectrometry Society, 2014, 35(2): 170-178. DOI: 10.7538/zpxb.2014.35.02.0170

Simultaneous Determination of the Estrogen, Progestogen and Androgen in Aquatic Products by Isotope Dilution LC-MS/MS

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  • A method of liquid chromatography-tandem mass spectrometry(LC-MS/MS) was developed for the simultaneous determination of estrogen, progestogen and androgen in aquatic products muscle tissues. The sample were extracted by tert-butyl methyl ether and ethyl acetate, purified on C18 solid phase extraction column, eluted by methanol. After XBridge RP-18 column separation using 0.02% ammonia-methanol as mobile phase, the eluents were qualitatively and quantitatively determined under multi-reaction monitoring scan type with tandem mass analyzer using positive polarity mode for the progestogen, androgen and estradiol benzoate, negative polarity for the estrogen respectively, the quantification was performed with internal standard method. The limit of detection is 0.5—2 μg/kg(S/N≥3). Spike recoveries are 73.0%—120% and 79.0%—108% in 2 μg/kg and 10 μg/kg with relative standard deviation of 5.3%—15% and 2.3%—8.2%. The method is effective, simple and sensitive, and suitable for the determination and confirmation of 27 kinds of sex hormones in aquatic products.
  • [1]
    虞淼,吴淑春.食品中性激素多组分残留分析方法的概述[J].食品工业科技,2010, 31(2):378-379.YU Miao, WU Shuchun. Review of residual multi-component analytical methods for the determination of steroid hormones in foods[J]. Science and Technology of Food Industry, 2010, 31(2):378-379(in Chinese).
    [2]
    郁倩,王洪新,刘德成.食品中性激素残留及检测方法的研究进展[J].中国卫生检验杂志,2008,18(2):377-378.YU Qian, WANG Hongxin, LIU Decheng. Research progress of residues and detetction method for sexual hormones in foods[J]. Chinese Journal of Health Laboratory Technology, 2008,18(2):377-378(in Chinese).
    [3]
    农业部兽医局. 中华人民共和国农业部公告第235号[EB/OL].[2013-07-01]. http://www.moa.gov.cn/zwllm/nybz/200803/t20080304-1028649.htm.
    [4]
    TRINH T, HARDEN NICK B, COLEMAN H M, et al. Simultaneous determination of estrogenic and androgenic hormones in water by isotope dilution gas chromatography-tandem mass spectrometry[J]. Journal of chromatography A, 2011,1 218(12):1668-1676.
    [5]
    林维宣,董伟峰,陈溪,等.气相色谱-质谱法同时检测动物组织中多种激素类兽药的残留量[J].色谱,2009,27(3):294-298.LIN Weixuan, DONG Weifeng, CHEN Xi, et al. Determination of hormone multi-residues in animal tissues by gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, 2009,27(3):294-298(in Chinese).
    [6]
    王玉飞,周凯,李继革.GC/MS/MS法同时测定海产品中4种雌激素残留[J].中国卫生检验杂志,2006,16(1):21-23.WANG Yufei, ZHOU Kai, LI Juge. Determination of estrogens in marine foods by gas chromatography/mass /mass spectrometry[J]. Chinese Journal of Health Laboratory Technology, 2006,16(1):21-23(in Chinese).
    [7]
    邹龙,林洪,江洁.氘代同位素内标气相色谱-质谱法测定鱼贝类肌肉中β-雌二醇残留[J].分析化学,2007,7(35): 983-987. ZOU Long, LIN Hong, JIANG Jie. Determination of β-etradiol residues in fish/shellfish muscles tissues by gas chromatography-mass spectrometry[J]. Chinese Journal of Analytical Chemistry, 2007,7(35):983-987(in Chinese).
    [8]
    湛嘉,俞雪钧,李佐卿, 等.黄鳝肌肉中20种性激素同时测定的气质联用检测法[J].食品科学,2008,29(6):298-303.ZHAN Jia, YU Xuejun, LI Zuoqing, et al. Simultaneous determination of residue of sex hormones in eel muscle by gas chromatographymass spectrometry[J]. Food Science,2008,29(6):298-303(in Chinese).
    [9]
    湛嘉, 俞雪钧,李佐卿,等. 猪尿中26种性激素与13种β2-激动剂的同时测定[J].分析测试学报, 2009, 28(10): 1133-1137.ZHAN Jia, YU Xuejun, LI Zuoqing, et al. Determintion of sex hormones and β2-agonists multi-residue in porcine urine by gas chromatography-mass spectrometry method[J]. Journal of Instrumental Analysis, 2009,28(10):1133-1137(in Chinese).
    [10]
    林春晓,王起恩,刘开钳,等.保健食品中五种性激素的高效液相色谱测定法[J].中华预防医学杂志,2003, 37(4):275-277.LIN Chunxiao, WANG Qien, LIU Kaiqian, et al. Determination of five sexual hormones in health foods by high performance liquid chromatography[J].Chin J Prev Med, 2003,37(4):275-277(in Chinese).
    [11]
    王小芳,王菁,任韧,等.反相高效色谱法同时测定化妆品中的7种性激素[J].中国卫生检验杂志,2008,18(11):2199-2211.WANG Xiaofang, WANG Jing, REN Ren, et al. Simultaneous determination of seven sexual hormones in cosmetics by reversed-phase high performance liquid chromatography[J]. Chinese Journal of Health Laboratory Technology, 2008,18(11):2199-2211(in Chinese).
    [12]
    王小芳,曾文芳,王菁,等.高效液相色谱-二级管阵列/荧光检测器串联法同时测定精油中七种性激素[J].色谱,2009,27(3):328-332.WANG Xiaofang, CENG Wenfang, WANG Jing. Simultaneous determination of Seven sexual hormones in essential oil by high performance liquid chromatography with diode arry and fluorescence detectors[J]. Chinese Journal of Chromatography, 2009,27(3):328-332(in Chinese).
    [13]
    迂君,张秀丽,张玉黔. 高效液相色谱法测定牛奶中雌激素残留量[J]. 中国卫生检验杂志,2007,17(6):1139-1140.YU Jun, ZHANG Xiuli, ZHANG Yuqian. Determination of estrogens in milk by high performance liquid chromatography[J]. Chinese Journal of Health Laboratory Technology, 2007,17(6):1139-1140(in Chinese).
    [14]
    徐英江,田秀慧,张秀珍,等.超高效液相色谱串联质谱法对水产品中8种雌激素的测定[J].分析测试学报,2010, 29(2):152-156.XU Yingjiang, TIAN Xiuhui, ZHANG Xiuzhen, et al. Determination of 8 estrogens in aquatic producte by ultra performance liquid chromatography-tandem mass spectrometry[J]. Journal of Instrumental Analysis, 2010, 29(2):152-156 (in Chinese).
    [15]
    张爱芝,王全林,沈坚,等.超高效液相色谱串联质谱法同时测定鱼制品中残留的7种性激素[J].色谱,2010, 28(2):190-196.ZHANG Aizhi, WANG Quanlin, SHEN Jian, et al. Simultaneous determination of seven hormones in fish products using ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2010, 28(2):190-196 (in Chinese).
    [16]
    秦燕,陈捷,张美金.动物肌肉组织中甾类同化激素多组分残留的液相色谱-质谱检测方法[J].分析化学,2006, 34(3):298-302.QIN Yan, CHEN Jie, ZHANG Meijin, Determination of anabolic hormones multrresidues in animal muscle tissues using liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Analytical Chemistry, 2006, 34(3):298-302 (in Chinese).
    [17]
    王全林,张爱芝,陈立仁. 超高效液相色谱-串联质谱法对奶制品中苯甲酸雌二醇残留的测定[J]. 分析测试学报, 2009, 28(9): 1069-1073.WANG Quanlin, ZHANG Aizhi, CHEN Liren. Determination of estradiol benzoate residues in dairy products by ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry[J]. Journal of Instrumental Analysis, 2009, 28(9): 1069-1073 (in Chinese).
    [18]
    DUFFY E, RAMBAUD L, BIZEC B L, et al. Determination of hormonal growth promoters in bovine hair: Comparison of liquid chromatography-mass spectrometry and gas chromatography-mass spectrometry methods for estradiol benzoate and nortestosterone decanoate[J]. Analytica Chimica Acta, 2009, 637(1/2): 165-172.
    [19]
    YANG Yi, SHAO Bing, ZHANG Jing, et al. Determination of the residues of 50 anabolic hormones in muscle, milk and liver by very-high-pressure liquid chromatography-electrospray ionization tandem mass spectrometry[J]. Journal of Chromatography B, 2009, 877(5/6): 489-496.
    [20]
    孙汉文,康占省,李挥. 凝胶渗透色谱-固相萃取净化-超快速液相色谱-串联质谱法检测牛肉中9种类固醇激素残留[J].分析化学, 2010, 38(9): 1272-1276.SHUN Hanwen, KANG Zhansheng, LI Hui. Determination of nine steriod hormones residues in beef sample by gel permeation chromatography-solid phase extraction-rapid resolution liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Analytical Chemistry, 2010, 38(9): 1272-1276 (in Chinese).
    [21]
    丛培福,柯润辉,程劲松.超高压液相色谱-串联质谱法测定乳制品中性激素类兴奋剂多残留的研究[J].食品安全质量检测学报, 2007, 27(1):36-42.CONG Peifu, KE Runhui, CHENG Jinsong, Determination of sex hormones residues in milk products by ultra performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety and Quality, 2007, 27(1):36-42 (in Chinese).
    [22]
    陈慧华,应永飞,吴平谷,等.液相色谱-串联质谱同时测定动物组织中22种同化激素[J].分析化学,2009,37(2):181-186.CHEN Huihua, YING Yongfei, WU Pinggu, et al. Multi-residue method for detrmination of 22 anabolic hormones in animal tissues by liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Analytical Chemistry, 2009,37(2):181-186(in Chinese).
    [23]
    GB/T 21981—2008 动物源性食品中激素多残留检测方法 液相色谱-质谱/质谱法[S].北京:中国标准出版社,2008.
    [24]
    赖世云,陶保华,傅士姗,等.液相色谱-质谱联用测定乳及乳制品中29种性激素[J].分析化学,2012, 40(1): 135-139.LAI Shiyun, TAO Baohua, FU Shishan, et al. Determination of 29 kinds of estrogens in milk and milk products by liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Analytical Chemistry, 2012, 40(1): 135-139 (in Chinese).

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