色谱

色谱 ›› 2013, Vol. 31 ›› Issue (10): 934-938.DOI: 10.3724/SP.J.1123.2013.01048

• 研究论文 • 上一篇    下一篇

超高效亲水色谱-串联质谱法快速检测鸡肉及其制品中的利巴韦林及其代谢物的总残留量

祝伟霞1, 杨冀州1, 袁萍1, 孙转莲1, 王彩娟2, 孙武勇1, 张书胜2   

  1. 1. 河南出入境检验检疫局, 河南 郑州 450003;
    2. 郑州大学化学与分子工程学院, 河南 郑州 450042
  • 收稿日期:2013-03-30 修回日期:2013-05-17 出版日期:2013-10-28 发布日期:2013-10-08
  • 通讯作者: 杨冀州
  • 基金资助:

    河南省科技攻关项目(122102110167)和质检总局科研项目(2007IK162).

Rapid determination of total residues of ribavirin and its metabolites in chicken and chicken products by ultra-performance hydrophilic interaction chromatography-tandem mass spectrometry

ZHU Weixia1, YANG Jizhou1, YUAN Ping1, SUN Zhuanlian1, WANG Caijuan2, SUN Wuyong1, ZHANG Shusheng2   

  1. 1. Henan Entry-Exit Inspection and Quarantine Bureau, Zhengzhou 450003, China;
    2. College of Chemistry and Molecular Engineering of Zhengzhou University, Zhengzhou 450042, China
  • Received:2013-03-30 Revised:2013-05-17 Online:2013-10-28 Published:2013-10-08

PDF

294

被引次数

23

摘要：

建立了鸡肉及其制品中利巴韦林和磷酸化利巴韦林代谢物总残留量的亲水作用色谱-串联质谱分析方法(HILIC-MS/MS)。样品采用含1%(v/v)乙酸的乙腈超声提取,于37 ℃条件下以酸性磷酸酶酶解,正己烷除脂后用C18与PSA填料分散固相萃取净化。采用酰胺基超高效亲水作用色谱柱,在乙腈和0.1%甲酸组成的梯度洗脱流动相中分离,在电喷雾正离子电离多反应监测模式下监测,结果表明,样品中利巴韦林残留量在1~200 μg/kg之间时,线性相关系数大于0.999,方法检出限(LOD, S/N≥3)为1 μg/kg,定量限(LOQ, S/N≥10)为5 μg/kg,在3个添加水平下的回收率为67.8%~112.7%,相对标准偏差为6.1%~13.6%。经测定多种实际样品,证明该方法简便、快速、准确,可以满足日常鸡肉及其制品中利巴韦林及其代谢物总残留量的分析要求。

关键词: 分散固相萃取, 鸡肉制品, 利巴韦林, 亲水色谱, 速成鸡, 液相色谱-串联质谱

Abstract:

An analytical method was developed for the determination of total residues of ribavirin and its phosphorylated metabolites in chicken and its products by hydrophilic interaction chromatography-tandem mass spectrometry. The samples were extracted with acetonitrile containing 1% (v/v) acetic acid under ultrasonic condition and then enzymatically hydrolysed with acid phosphatase at 37 ℃. After liposoluble substances being removed with hexane, C18 and PSA dispersion solid phase extraction (DSPE) was introduced to cleanup procedures. The separation was performed on an ultra-performance hydrophilic interaction chromatographic (HILIC) amide column under a gradient elution using acetonitrile and 0.1% formic acid. The analytes were detected in the positive electrospray ionization and multi-reaction monitoring (MRM) mode. In the range of 1-200 μg/kg, the correlation coefficient was greater than 0.999. The limit of detection (LOD, S/N≥3) was 1 μg/kg and the limit of quantification (LOQ, S/N≥10) was 5 μg/kg. The recoveries of ribavirin spiked at three levels ranged from 67.8% to 112.7% with the relative standard deviations (RSDs) of 6.1%-13.6%. The results of the determination of ribavirin in various real samples showed that the method is simple, rapid, accurate and suitable for the determination of total residues of ribavirin and its metabolites in chicken and its products.

Key words: chicken products, dispersion solid phase extraction (DSPE), hydrophilic interaction chromatography (HILIC), liquid chromatography-tandem mass spectrometry (LC-MS/MS), quick growth chicken, ribavirin

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