液相色谱串联质谱法测定水产品中苯甲酸雌二醇的残留

doi:10.7506/spkx1002-6630-201322042

食品科学 ›› 2013, Vol. 34 ›› Issue (22): 208-211.doi: 10.7506/spkx1002-6630-201322042

液相色谱串联质谱法测定水产品中苯甲酸雌二醇的残留

张珊珊，于慧娟，惠芸华，冯兵，张晓玲

1.上海海洋大学食品学院，上海 201306；
2.中国水产科学研究院东海水产研究所，水产品质量安全加工实验室，上海 200090

收稿日期:2013-07-01 修回日期:2013-10-11 出版日期:2013-11-25 发布日期:2013-12-05
通讯作者: 于慧娟 E-mail:yuhuijuan607@sohu.com
基金资助:
农业部行业标准制定项目

Determination of Estradiol Benzoate Residues in Aquatic Products by LC-MS-MS

ZHANG Shan-shan，YU Hui-juan，HUI Yun-hua，FENG Bing，ZHANG Xiao-ling

1. College of Food Science and Technology, Shanghai Ocean University, Shanghai 201306, China；
2. Laboratory of Aquatic Products Quality Safety and Processing, East China Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences, Shanghai 200090, China

Received:2013-07-01 Revised:2013-10-11 Online:2013-11-25 Published:2013-12-05
Contact: Yu Hui-Juan E-mail:yuhuijuan607@sohu.com

摘要/Abstract

摘要：

通过对前处理以及仪器方法的研究和优化，建立水产品中苯甲酸雌二醇残留的液相色谱串联质谱检测方法。样品经甲基叔丁基醚提取，LC-C18固相萃取小柱净化，甲醇-水溶液定容后离心去脂。采用甲醇-水为流动相，经Waters XBridge RP-18色谱柱(150mm×4.6mm，5μm)分离后，电喷雾串联质谱测定，以甲羟孕酮-D3为内标进行定量。在标准添加水平1～10μg/kg范围内，加标回收率为77.9%～113.5%，相对标准偏差不超过9.4%，定量限为1μg/kg。该方法灵敏度高，重复性好，适用于各种水产品中苯甲酸雌二醇残留量的测定。

关键词: 苯甲酸雌二醇, 水产品, 酶解, 液相色谱串联质谱

Abstract:

A high performance liquid chromatography-tandem mass spectrometric (LC-MS-MS) method has been
established for the determination of estradiol benzoate residues in aquatic products. Sample pretreatment conditions and
instrumental parameters were optimized. Samples were extracted with methyl tert-butyl ether, cleaned up on an LC-C18 solid
phase extraction column and degreased with methanol-water. Separation of the analyte was carried out on Waters XBridge
RP-18 column (150 mm × 4.6 mm i.d., 5 μm) using a mobile phase made up of methanol and water before analysis by
electrospray ionization LC-MS-MS using medroxyprogesterone-D3 as internal standard. The limit of quantification of this
method was 1 μg/kg. The average recovery from samples spiked in the range of 1 to 10 μg/kg was 77.9%–113.5%, with
RSD less than 9.4%. This method was sensitive, reproducible, and suitable for the determination of estradiol benzoate in
various aquatic products.

Key words: estradiol benzoate, aquatic products, enzymatic hydrolysis, high performance liquid chromatographytandem mass spectrometry (LC-MS-MS)

中图分类号:

TS254

张珊珊，于慧娟，惠芸华，冯兵，张晓玲. 液相色谱串联质谱法测定水产品中苯甲酸雌二醇的残留[J]. 食品科学, 2013, 34(22): 208-211.

ZHANG Shan-shan，YU Hui-juan，HUI Yun-hua，FENG Bing，ZHANG Xiao-ling. Determination of Estradiol Benzoate Residues in Aquatic Products by LC-MS-MS[J]. FOOD SCIENCE, 2013, 34(22): 208-211.

参考文献

[1] HOOIJERINK H, LOMMEN A, MULDER P P J, et al. Liquid chromatography–electrospray ionisation-mass spectrometry based method for the determination of estradiol benzoate in hair of cattle[J]. Analytica Chimica Acta, 2005, 529: 167-172.

[2] 杨永铨, 张中英, 林克宏, 等. 莫桑比克罗非鱼性别生理遗传控制的初步研究[J]. 遗传学报, 1979, 6(3):305-310.

[3] 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.

[4] 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: 165-172.

[5] 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: 489-496.

[6] 邹龙. 气相色谱质谱联用技术对水产品中激素多残留检测的研究[D]. 青岛: 中国海洋大学, 2008.

[7] 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.

[8] 湛嘉, 俞雪钧, 李佐卿, 等. 黄鳝肌肉中11种性激素的气质联用检测方法[J]. 分析测试学报, 2007, 26(5): 642-646.

[9] 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]. 分析化学研究报告, 2010, 38(9): 1272-1276.

[10] BLASCO C, POUCKE C V, PETEGHEM C V. Analysis of meat samples for anabolic steroids residues by liquid chromatography/tandem mass spectrometry. Journal Chromatography A. 2007, 1154: 230-239.

[11] SANGIORGI E, CURATOLO M, ASSINI W, et al. Apllication of neutral loss mode in liquid chromatography-mass spectrometry for the determination of corticosteroids in bovine urine[J]. Analytica Chimica Acta, 2003, 483: 73-86.

[12] SHAO Bing, ZHAO Rong, MENG Juan, et al. Simultaneous determination of residual hormonal chemicals in meat, kidney, liver tissues and milk by liquid chromatography-tandem mass spectrometry[J]. Analytica Chimica Acta, 2005, 548: 41-50.

[13] DUNN T G, KALTENBACH C C, KORITNIK D R, et al. Metabolites of estradiol-17βand estradiol-17β-3-benzoate in bovine tissues[J]. Journal of Animal Science, 1977, 45: 659-673.

[14] ESTERGREEN V L, LIN M T, MARTIN E L, et al. Distribution of progesterone and its metabolites in cattle tissues following administration of progesterone-4-14C1,2,3,4[J]. Journal of Animal Science, 1977, 45: 642-651.

[15] HOFFMANN B, RATTENBERGER E. Testosterone concentrations in tissue from veal calves, bulls and heifers and in milk-samples[J]. Journal of Animal Science, 1977, 45: 635-641.

[16] VANHAECKE L, BUSSCHE V J, WILLE K, et al. Ultra-high performance liquid chromatography–tandem mass spectrometry in high-throughput con?rmation and quanti?cation of 34 anabolic steroids in bovine muscle[J]. Analytica Chimica Acta, 2011, 700: 70-77.

[17] 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]. 分析化学研究报告, 2012, 40(1): 135-139.

[18] ZENG Dongping, LIN Cuiping, ZENG Zhe-ling, et al. Multi-residue determination of eight anabolic steroids by GC-MS in muscle tissues from pigs[J]. Agricultural Sciences in China, 2010, 9(2): 306-312.

[19] 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]. 分析化学研究报告, 2009, 37(2): 181-186.

[20] KOOTSTRA P R, ZOONTJES P W, TRICHT E F, et al. Multi-residue screening of a minimum package of anabolic steroids in urine with GC–MS[J]. Analytica Chimica Acta, 2007, 586: 82-92.

液相色谱串联质谱法测定水产品中苯甲酸雌二醇的残留

Determination of Estradiol Benzoate Residues in Aquatic Products by LC-MS-MS

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