色谱

色谱

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定饲料中的维吉尼霉素M1

黄永辉*   

  1. 福建省产品质量检验研究院, 国家加工食品质量监督检验中心, 福建 福州 350002
  • 收稿日期:2011-04-08 修回日期:2011-05-09 出版日期:2011-10-28 发布日期:2011-10-13
  • 通讯作者: 黄永辉,工程师. Tel: （0591）83762000,
  • 基金资助:
    福建省质量技术监督局科技计划项目(FJQI2009018)

Determination of virginiamycin M1 in feeds by ultra high performance liquid chromatography-tandem mass spectrometry

HUANG Yonghui*   

  1. National Quality Supervision and Testing Center for Processed Food, Fujian Inspection and Research Institute for Product Quality, Fuzhou 350002, China
  • Received:2011-04-08 Revised:2011-05-09 Online:2011-10-28 Published:2011-10-13

PDF

547

被引次数

18

摘要： 建立了饲料中维吉尼霉素M1的超高效液相色谱-串联质谱(UPLC-MS/MS)分析测定方法。样品用乙腈-0.2%(v/v)甲酸水溶液(8:2, v/v)超声提取两遍后,通过UPLC-MS/MS进行分析,以BEH C18色谱柱为分析柱,乙腈-0.3%(v/v)甲酸水溶液（35:65, v/v）为流动相,采用电喷雾电离正离子模式,以多反应监测模式进行定性和定量分析。在0.3～226.6 μg/L范围内线性关系良好(相关系数r=0.9995)。维吉尼霉素M1的检出限和定量限分别为2 μg/kg和7 μg/kg,平均回收率为82.6%～102.7%,相对标准偏差为0.9%～10.5%。结果表明,该方法具有操作简单、准确度和灵敏度高、重现性好的特点,适合用于检测饲料中维吉尼霉素M1的含量。

null

关键词: 超高效液相色谱-串联质谱, 饲料, 维吉尼霉素M1

Abstract: A comprehensive analytical method based on ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been developed for the determination of virginiamycin M1 in feeds. The sample was extracted twice by ultrasonic extraction with acetonitrile-0.2% (v/v) formic acid (8:2, v/v). The chromatographic separation was achieved with a BEH C18 column and acetonitrile-0.3%(v/v) formic acid （35:65, v/v） as the mobile phase. The identification and quantification of the analyte were carried out on electrospray ionization MS/MS in a multiple reaction monitoring (MRM) mode. The correlation coefficient (r) of virginiamycin M1 was 0.9995 in the linear range of 0.3~226.6 μg/L. The detection limit (S/N=3) and quantification limit (S/N=10) of virginiamycin M1 were 2 μg/kg and 7 μg/kg, respectively. The average spiked recoveries were in the range of 82.6% to 102.7% with the relative standard deviations (RSDs) of 0.9%~10.5%. The results demonstrate that the proposed method is simple, sensitive, repeatable and suitable for the testing of virginiamycin M1 in feeds.

Key words: feeds, ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), virginiamycin M1