色谱

色谱 ›› 2013, Vol. 31 ›› Issue (9): 862-868.DOI: 10.3724/SP.J.1123.2013.02026

• 研究论文 • 上一篇    下一篇

分散固相萃取-超高效液相色谱-串联质谱法同时检测火锅食材中11种喹诺酮类药物

曹鹏1, 牟妍1, 高飞2, 耿金培1, 张禧庆3, 隋涛1, 梁君妮1, 沙美兰1, 关丽丽1   

  1. 1. 烟台出入境检验检疫局, 山东 烟台 264000;
    2. 青岛出入境检验检疫局, 山东 青岛 266000;
    3. 烟台杰科检测服务有限公司, 山东 莱阳 265231
  • 收稿日期:2013-02-25 修回日期:2013-04-19 出版日期:2013-09-28 发布日期:2013-09-02
  • 通讯作者: 曹鹏
  • 基金资助:

    山东检验检疫局科技计划项目(SK201173);烟台市科技发展计划项目(2011052).

Simultaneous determination of 11 quinolones in hotpot ingredients by dispersive solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry

CAO Peng1, MOU Yan1, GAO Fei2, GENG Jinpei1, ZHANG Xiqing3, SUI Tao1, LIANG Junni1, SHA Meilan1, GUAN Lili1   

  1. 1. Yantai Entry-Exit Inspection and Quarantine Bureau, Yantai 264000, China;
    2. Qingdao Entry-Exit Inspection and Quarantine Bureau, Qingdao 266000, China;
    3. Yantai Jieke Inspection Service Co., Ltd., Laiyang 265231, China
  • Received:2013-02-25 Revised:2013-04-19 Online:2013-09-28 Published:2013-09-02

PDF

278

被引次数

37

摘要：

建立了一种固相分散萃取-超高效液相色谱-串联质谱(QuEChERS-UPLC-MS/MS)同时检测火锅食材中11种喹诺酮类药物的方法。样品用5%甲酸乙腈溶液提取后加入盐析剂分层,提取液中加入C18和PSA填料进行基质分散固相净化,浓缩后经Poroshell 120 EC-C18柱分离,用电喷雾离子源正离子多反应监测(MRM)模式串联质谱进行检测。11种药物在1.0~100.0 μg/kg范围内具有较好的线性关系,相关系数均大于0.998。该方法检出限(LOD)为1.8~3.1 μg/kg,定量限(LOQ)为6.0~10.3 μg/kg。11种药物的回收率为70.1%~100.3%,相对标准偏差(RSD)为2.42%~10.88%。该方法简便快速、灵敏度高、准确度好、使用范围广,可作为火锅食材中11种喹诺酮类药物残留的确证方法。

关键词: 超高效液相色谱-串联质谱, 分散固相萃取, 火锅食材, 喹诺酮类药物

Abstract:

A method for the simultaneous determination of the residues of 11 quinolones in hotpot ingredients by quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction and ultra performance liquid chromatography-tandem mass spectrometric method (UPLC-MS/MS) was established. The sample was extracted with acetonitrile (containing 5% formic acid) and followed by stratifying with a salting-out agent. Clean-up of the extracts was processed by C18 and PSA, a modified QuEChERS procedure. The analytes were then separated on a Poroshell 120 EC-C18 column, and finally detected by tandem mass spectrometry in positive ESI mode. The linearity of all the 11 quinolones in the range from 1.0 to 100.0 μg/kg had correlation coefficients greater than 0.998. The limits of detection (LOD) of the method were from 1.8 to 3.1 μg/kg and the limits of quantification (LOQ) were from 6.0 to 10.3 μg/kg. The average recoveries of the 11 quinolones were in the range from 70.1% to 100.3%, with relative standard deviations from 2.42% to 10.88%. The established method is sensitive and of good recoveries. It can be applied as a rapid and reliable method for the determination of the 11 quinolones in hotpot ingredients.

Key words: hotpot ingredients, QuEChERS, quinolones, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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