色谱

色谱

• 研究论文 • 上一篇    下一篇

液相色谱-电喷雾串联质谱法测定禽类产品中克球酚的残留

杨雯筌1*,徐锦忠1,杨功俊2,丁涛1,齐涓菲2,柳菡1,沈崇钰1,吴斌1,余枢1   

  1. 1.Laboratory of Food, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China; 2.School of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou 225009, China
  • 收稿日期:2008-08-25 修回日期:2008-10-25 出版日期:2009-03-30 发布日期:1982-12-25
  • 通讯作者: 杨雯筌
  • 基金资助:
    科技部质检公益项目(200810099)

Determination of clopidol residue in poultry products by liquid chromatography-electrospray ion trap tandem mass spectrometry

YANG Wenquan1*, XU Jinzhong1, YANG Gongjun2, DING Tao1, QI Juanfei2, LIU Han1, SHEN Chongyu1, WU Bin1, YU Shu1   

  1. 1.Laboratory of Food, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China; 2.School of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou 225009, China
  • Received:2008-08-25 Revised:2008-10-25 Online:2009-03-30 Published:1982-12-25
  • Contact: YANG Wenquan

PDF

720

被引次数

23

摘要： 建立了禽类产品中克球酚残留的液相色谱-电喷雾串联质谱(LC-ESI-MS/MS)检测方法。用甲醇对样品进行提取,提取液用正己烷萃取去油脂,然后用LC-18柱和阴离子交换柱净化,LC-ESI-MS/MS测定。利用基质校正曲线对克球酚准确定量。在2,5,10,20 μg/kg 4个添加水平下,克球酚的平均回收率稳定在55.38%～132.44%之间,日内精密度小于9.54%,日间精密度小于15.27%。在1～40 μg/kg范围内色谱峰面积与克球酚含量呈良好的线性关系,检出限为0.5 μg/kg，定量限为2.0 μg/kg。该方法选择性好,抗干扰能力强,可作为禽类产品中克球酚残留检测的确证方法。

关键词: 固相萃取, 基质效应 , 克球酚, 禽类产品, 液相色谱-电喷雾串联质谱联用

Abstract: A method is presented for the determination of clopidol residue in poultry products by liquid chromatography-electrospray ion trap tandem mass spectrometry (LC-ESI-MS/MS). Clopidol residue was extracted with methanol and cleaned-up by n-hexane from different poultry products. The extract was cleaned-up by an LC-18 column and an ion exchange solid phase extraction (SPE) column. Quantification was achieved by matrix calibration. The recoveries of clopidol in poultry products were in the range from 55.38% to 132.44% at the four spiked levels, 2, 5, 10, and 20 μg/kg. The intra-day relative standard deviation (RSD) and inter-day RSD were less than 9.54% and 15.27%, respectively. The linearity of the method was good from 1 μg/kg to 40 μg/kg. The limit of detection (LOD) was 0.5 μg/kg, and the limit of quantification (LOQ) was 2.0 μg/kg. The method is selective without interference and suitable for the determination and confirmation of clopidol residue in poultry products.

Key words: clopidol, matrix effect , poultry products, solid phase extraction (SPE), liquid chromatography-electrospray ion trap tandem mass spectrometry (LC-ESI-MS/MS)