色谱

色谱

• 研究论文 • 上一篇    下一篇

气相色谱-质谱法测定动物组织中三种1,2-二苯乙烯类药物的残留量

吴银良1,2,刘素英1,侯东军1,沈建忠2,王海1,单吉浩1   

  1. 1.Quality Control and Inspection Center for Domestic Animal Products of Ministry of Agriculture, Beijing 100026, China; 2.College of Veterinary Medicine, China Agricultural University, Beijing 100094, China
  • 收稿日期:2005-11-30 修回日期:2006-05-24 出版日期:2006-09-30 发布日期:1986-09-25
  • 通讯作者: 吴银良

Determination of Residues of Three Stilbene Drugs in Animal Tissues Using Gas Chromatography-Mass Spectrometry

WU Yinliang1,2, LIU Suying1, HOU Dongjun1, SHEN Jianzhong2, WANG Hai1, SHAN Jihao1   

  1. 1.Quality Control and Inspection Center for Domestic Animal Products of Ministry of Agriculture, Beijing 100026, China; 2.College of Veterinary Medicine, China Agricultural University, Beijing 100094, China
  • Received:2005-11-30 Revised:2006-05-24 Online:2006-09-30 Published:1986-09-25
  • Contact: Wu Yinliang

PDF

615

被引次数

17

摘要： 建立了动物组织中己烯雌酚(DES)、己二烯雌酚(DIS)和己烷雌酚(HS)残留量的气相色谱-质谱分析方法。动物组织样品在碱性条件下用乙酸乙酯提取,经碳酸钠溶液液-液分配净化,再用硅胶柱固相萃取净化,洗脱液均分成两份后经氮气吹干,分别用双三甲基硅基三氟乙酰氨(BSTFA)和七氟丁酸酐(HFBA)衍生,采用选择离子监测模式(SIM)进行测定,外标法定量。检出限为0.30 μg/kg(cis-DES)，0.10 μg/kg(trans-DES和HS)和0.15 μg/kg(DIS)。在0.5~4.0 μg/kg添加水平,回收率为73.0%～86.5%,相对标准偏差(RSD)为1.0%～7.2%。衍生物的峰面积与样品浓度在10～1000 μg/L(DES和DIS) 和5～500 μg/L(HS)范围内呈良好的线性关系,线性回归系数大于0.99。

关键词: 1,2-二苯乙烯类药物, 残留, 动物组织 , 固相萃取, 气相色谱, 质谱

Abstract: A method has been developed to determine residual stilbenes such as diethylstilbestrol (DES), dienestrol (DIS) and hexestrol (HS) in animal tissues using solid phase extraction (SPE) and gas chromatography-mass spectrometry (GC-MS). The procedures for extraction, cleanup on an LC-Si solid phase extraction cartridge and derivatization of stilbenes were established and optimized. The analytes were detected by mass spectrometer with electron impact source in selected ion monitoring mode(EI/SIM), and quantified with an external standard calibration curve method. Linear calibration curves were obtained in the concentration ranges from 5 to 500 μg/L for HS and from 10 to 1 000 μg/L for DES and DIS(the correlation coefficients were above 0.99). Recoveries of the stilbenes were 73.0%-86.5%, and the relative standard deviations were between 1.0% and 7.2%. The limits of detection were 0.30 μg/kg for cis-DES, 0.10 μg/kg for trans-DES and HS and 0.15 μg/kg for DIS in pork and swine liver.

Key words: animal tissues , gas chromatography (GC), mass spectrometry (MS), residue, stilbenes, solid phase extraction (SPE)