色谱

色谱

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蛋品中苏丹红残留的液相色谱串联质谱测定法研究

王鹏1,2,郭少飞3,荆涛1,胡小钟2,林雁飞2,罗静2,宋祺2,周宜开1,梅素容1

  

  1. 1.Institute of Environmental Medicine, School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, Key Laboratory of Environment &Health of Ministry of Education, Wuhan 430030, China; 2.Hubei Entry-Exit Inspection and Quarantine Bureau, Wuhan 430022, China; 3.Pharmacy College, Tongji Medical College, Huazhong University, Wuhan 430030, China
  • 收稿日期:2007-09-13 修回日期:2007-11-06 出版日期:2008-05-30 发布日期:1984-03-25
  • 通讯作者: 梅素容

Determination of Sudan Residues in Eggs by Liquid Chromatography Tandem Mass Spectrometry

WANG Peng1,2, GUO Shaofei3, JING Tao1, HU Xiaozhong2, LIN Yanfei2, LUO Jing2, SONG Qi2, ZHOU Yikai1, MEI Surong1   

  1. 1.Institute of Environmental Medicine, School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, Key Laboratory of Environment &Health of Ministry of Education, Wuhan 430030, China; 2.Hubei Entry-Exit Inspection and Quarantine Bureau, Wuhan 430022, China; 3.Pharmacy College, Tongji Medical College, Huazhong University, Wuhan 430030, China
  • Received:2007-09-13 Revised:2007-11-06 Online:2008-05-30 Published:1984-03-25

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摘要： 采用液相色谱-串联质谱法（LC-MS/MS）测定了蛋品中苏丹红I、II、III、Ⅳ号染料的残留。制样后，装柱，应用基质固相分散技术，用氯仿、乙腈混合溶液（体积比为90：10）淋洗，浓缩定容后经ZORBAX SB-C18柱分离，采用电喷雾正离子，多反应监控（MRM）模式检测。外标曲线定量，苏丹红I、II、III、Ⅳ的线性范围分别为0.5～100ng/g，5.0～100ng/g，1.0～100ng/g和2.0～100ng/g，线性方程的相关系数都大于0.99，添加样品回收率在87.3～113％之间，相对标准偏差均小于9.1％。针对四种苏丹红染料，该方法的检测低限分别可达0.1μg/kg，2.0μg/kg，0.2μg/kg，0.4μg/kg，可以满足国内外蛋品中苏丹红监控要求。

关键词: 基质固相分散技术, 禽蛋 , 苏丹红染料, 液相色谱-串联质谱法

Abstract: A new method was established for determining Sudan Ⅰ- Ⅳ in eggs by liquid chromatography tandem mass spectrometry (LC-MS/MS). The targeted analytes in eggs were extracted by solid-phase disperse technique with a mixture of chloroform and acetonitrile (9:1,v:v). Chromatographic separation was achieved by using ZORBAX SB-C18 column. Identification and quantification were performed using multiple- reaction monitoring (MRM) and electrospray ionization in positive mode. The linearity range of Sudan Ⅰ- Ⅳ was 0.5～100ng/g, 5.0～100ng/g，1.0～100ng/g and 2.0～100ng/g, respectively, and r>0.99. The recovery of determination of Sudan residues in eggs was between 87.3 %-113 % with RSD less than 9.1 %. The detection limit of this method was 0.1μg/kg (Ⅰ), 2.0μg/kg (II), 0.2μg/kg (III) and 0.4μg/kg (Ⅳ), respectively, which could meet the requirement of the Sudan residues monitoring both abroad and home.

Key words: Eggs, Liquid Chromatography tandem mass Spectrometry (LC-MS/MS), Solid-phase disperse technique , Sudan