色谱

色谱 ›› 2018, Vol. 36 ›› Issue (10): 999-1004.DOI: 10.3724/SP.J.1123.2018.05028

• 研究论文 • 上一篇    下一篇

QuEChERS-超高效液相色谱-串联质谱法检测羊肉中8种抗真菌药

张凯1,2, 秦宇2, 卞华2, 曹慧1, 刘天益2, 葛宇2   

  1. 1. 上海理工大学医疗器械与食品学院, 上海 200093;
    2. 上海市质量监督检验技术研究院, 上海 200233
  • 收稿日期:2018-05-31 出版日期:2018-10-08 发布日期:2014-08-22
  • 通讯作者: 葛宇.Tel:(021)64851815,E-mail:geyu@sqi.org.cn
  • 基金资助:

    上海市科技兴农重点攻关项目（沪农科攻字（2016）第4-5号）.

Determination of eight antifungal drugs in mutton by QuEChERS coupled with ultra-performance liquid chromatography-tandem mass spectrometry

ZHANG Kai1,2, QIN Yu2, BIAN Hua2, CAO Hui1, LIU Tianyi2, GE Yu2   

  1. 1. College of Medical Equipment and Food, University of Shanghai for Science and Technology, Shanghai 200093, China;
    2. Shanghai Institute of Quality Inspection and Technical Research, Shanghai 200233, China
  • Received:2018-05-31 Online:2018-10-08 Published:2014-08-22
  • Supported by:

    Shanghai Science and Technology Prosperous Agriculture Key Project (Chinese Characters of Shanghai Agricultural Sciences (2016) No. 4-5)

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摘要：

建立了QuEChERS-超高效液相色谱-串联质谱（UPLC-MS/MS）检测羊肉中8种抗真菌药的方法。羊肉样品用含2.0%（体积分数）甲酸的乙腈溶液提取后，采用QuEChERS方法净化。采用Atiantis® T3色谱柱（100 mm×2.1 mm，3 μm）进行分离，以乙腈-0.1%（v/v）甲酸水溶液为流动相进行梯度洗脱，在电喷雾电离源、正离子模式（ESI+）和多反应监测模式（MRM）下进行定性定量分析。实验比较了不同提取溶剂的提取效果，并优化了色谱和质谱的分析条件。结果表明，8种抗真菌药物在0.2~50 μg/L范围内线性关系良好，相关系数（R2）均>0.99；检出限（LOD）为0.3~3.0 μg/kg，定量限（LOQ）为1.0~10.0 μg/kg。8种抗真菌药在低、中、高3个水平下的平均加标回收率为70.3%~118.4%，相对标准偏差（RSD）为0.4%~4.3%（n=6）。该方法灵敏高效，回收率优良，重复性好，适用于羊肉样品抗真菌药物的有效检测。

关键词: QuEChERS, 超高效液相色谱-串联质谱, 抗真菌药, 羊肉

Abstract:

A method for the simultaneous determination of eight antifungal drugs in mutton was developed using QuEChERS combined with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were shaken with acetonitrile containing 2.0% (v/v) formic acid, and then subjected to QuEChERS purification. The residual targets were analyzed on an Atiantis® T3 column (100 mm×2.1 mm, 3 μm) with gradient elution using acetonitrile-0.1% (v/v) formic acid aqueous solution as the mobile phase. All the analytes were effectively separated and cleaned up within 9 min, and were finally detected by UPLC-MS/MS with ESI+ ionization in multiple reaction monitoring (MRM) mode. All the eight antifungal drugs showed a good linear trend in the range of 0.2-50 μg/L, with the correlation coefficient (R2) greater than 0.99. The limits of detection (LODs) and limits of quantification (LOQs) were 0.3-3.0 μg/kg and 1.0-10.0 μg/kg, respectively. The calibration curves were used in the analysis to reduce the negative influence of matrix effects. The average recoveries at different levels (low, medium, and high) for all the analytes ranged from 70.3% to 118.4%, with the relative standard deviations of 0.4%-4.3% (n=6). The developed method shows excellent recovery and stable repeatability, and is suitable for the determination of the antifungal drugs in mutton.

Key words: antifungal drugs, mutton, QuEChERS, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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