色谱

色谱

• 研究论文 • 上一篇    下一篇

固相萃取-液相色谱-质谱/质谱法同时测定蜂蜜中的多类药物残留

侯建波1,2, 谢文1,2*, 陈笑梅1,2, 奚君阳3, 钱艳3, 王峰3, 刘海山1,2   

  1. 1. 浙江出入境检验检疫局技术中心, 浙江 杭州 310016; 2. 浙江省检验检疫科学技术研究院, 浙江 杭州 310016; 3. 浙江立德产品技术有限公司, 浙江 杭州 310016
  • 收稿日期:2011-01-28 修回日期:2011-03-17 出版日期:2011-06-28 发布日期:2011-07-25
  • 通讯作者: 谢文,硕士,研究员,主要研究方向为食品中兽药残留检测. Tel: (0571)81100817,
  • 基金资助:

    国家质检总局科技计划项目(2008IK167)

Determination of 41 hormones in cereal feeds by liquid chromatography-tandem mass spectrometry

HOU Jianbo1,2, XIE Wen1,2*, CHEN Xiaomei1,2, XI Junyang3, QIAN Yan3, WANG Feng3, LIU Haishan1,2   

  1. 1. Technic Center of Zhejiang Entry-Exit Inspection and Quarantine Bureau, Hangzhou 310016, China; 2. Zhejiang Academy of Science and Technology for Inspection and Quarantine, Hangzhou 310016, China; 3. Zhejiang Lead Product Technic Co., Ltd., Hangzhou 310016, China
  • Received:2011-01-28 Revised:2011-03-17 Online:2011-06-28 Published:2011-07-25

PDF

656

被引次数

26

摘要： 建立了采用固相萃取-液相色谱-质谱/质谱(SPE-LC-MS/MS)对蜂蜜中磺胺类、硝基咪唑类、喹诺酮类、大环内酯类、林可酰胺类和吡喹酮共计6大类54种药物残留同时测定的方法。蜂蜜经磷酸盐缓冲溶液(pH 8)稀释,Oasis HLB固相萃取柱净化后,通过液相色谱-质谱联用技术进行检测(正离子方式,多反应监测模式)。采用同位素稀释内标法或外标法进行定量,线性关系良好,相关系数大于0.992。方法的定量限(LOQ,以信噪比(S/N)大于10计)分别为磺胺类和硝基咪唑类药物1.0 μg/kg,喹诺酮类和林可酰胺类药物2.0 μg/kg,大环内酯类药物3.0 μg/kg,吡喹酮0.3 μg/kg。总体回收率为32.6%～114%,相对标准偏差为1.3%～28.9%。该方法的定量限满足目前国内外药物的最大残留限量要求,可作为蜂蜜中相关药物残留量的筛选检测方法。

关键词: 多类药物残留, 蜂蜜, 液相色谱-质谱/质谱法

Abstract: A method was developed for the determination of 10 androgens, 11 progesterones, 10 glucocorticoids, 5 estrogens and 5 resorcylic acid lactones in cereal feeds by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Ethyl acetate was used to extract the sample, and the mixed QuEChERS sorbents were dispersed for purification. The extract was separated by a C18 column and detected in positive or negative multiple reaction monitoring (MRM) mode. With the optimal conditions, the linear ranges of 41 hormones were 5.0~200.0 μg/kg with the correlation coefficients above 0.99 and the limits of quantification (LOQs, S/N≥10) were 0.123~2.72 μg/kg. The method validation was carried out at three spiking levels, and the recoveries were 70.3%~118.1% for soybean meals with the relative standard deviations (RSDs) of 0.82%~19.5%, and 76.1%~122.8% for corn meals with the RSD of 1.3%~15.0%. This method is simple, fast and credible, can be applied to simultaneous screening and determination of estrogens, progesterones, androgens, glucocorticoids and resorcylic acid lactones belonging to the illegal additive of hormones in cereal feeds.

Key words: cereal feeds, estrogen, glucocorticoid, progesterone, resorcylic acid lactones, androgen, liquid chromatography-tandem mass spectrometry (LC-MS/MS)