食品科学 ›› 2018, Vol. 39 ›› Issue (18): 309-314.doi: 10.7506/spkx1002-6630-201818047

• 安全检测 • 上一篇    下一篇

不同前处理方法对猪组织中喹诺酮类兽药残留检测效果对比

王杰,裴斐,李彭,白宇杰,方勇,杨文建,马宁,胡秋辉*   

  1. (南京财经大学食品科学与工程学院,江苏省现代粮食流通与安全协同创新中心,江苏高校粮油质量安全控制及深加工重点实验室,江苏?南京 210023)
  • 出版日期:2018-09-25 发布日期:2018-09-18
  • 基金资助:
    江苏省农业科技自主创新资金项目(CX(16)1028);江苏高校优势学科建设工程资助项目(PAPD)

Comparison of Different Sample Pretreatments for the Analysis of Quinolone Residues in Porcine Tissues

WANG Jie, PEI Fei, LI Peng, BAI Yujie, FANG Yong, YANG Wenjian, MA Ning, HU Qiuhui*   

  1. (Key Laboratory of Grains and Oils Quality Control and Processing, Collaborative Innovation Center for Modern Grain Circulation and Safety, College of Food Science and Engineering, Nanjing University of Finance and Economics, Nanjing 210023, China)
  • Online:2018-09-25 Published:2018-09-18

摘要: 采用超高效液相色谱-三重四极杆质谱和飞行时间质谱技术,比较EMR-L、Oasis PRiME HLB和液液萃取法对猪组织中16?种喹诺酮类兽药残留检测效果的影响。目标兽药以基质匹配工作曲线进行定量,在1.0~100.0?μg/L范围内线性关系良好,在5、10、20?μg/kg加标量条件下使用超高效液相色谱-串联质谱检测,EMR-L和Oasis?PRiME?HLB方法处理的猪组织中加标回收率(71.7%~106.9%、70.7%~118.3%)、相对标准偏差(0.2%~16.8%、0.1%~17.8%)、定量限(0.13~0.56、0.27~1.36?μg/kg)和检出限(0.04~0.23、0.08~0.41?μg/kg)均满足方法学要求。针对不同基质成分样品,采用不同的前处理技术减少假阳性结果的产生,以适用于日益增长的动物源性食品兽药残留检测的需求。本研究采用的2?种方法操作简便、灵敏度高、重复性好,满足对猪组织中多兽药残留的定性、定量分析。

关键词: EMR-L, Oasis?PRiME?HLB, 液液萃取, 喹诺酮类, 猪组织

Abstract: This study investigated the influence of different sample pretreatments: enhanced matrix removal-lipid (EMR-L) for lipid, Oasis PRiME hydrophile lipophilic balance (HLB) and liquid-liquid extraction (LLE) on the assay of 16 quinolone residues in porcine tissues by ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry (UPLC-TQ-MS/MS) or quadrupole-time-of-flight tandem mass spectrometry (Q-TOF/MS). The target compounds were quantified by the matrix-matched calibration curve. Good linearity was observed for all analytes in the range of 1.0–100.0 μg/L. The recoveries using the EMR-L and Oasis PRiME HLB methods at spiked concentration levels (5, 10 and 20?μg/kg) were 71.7%–106.9% and 70.7%–118.3% with relative standard deviations of 0.2%–16.8% and 0.1%–17.8%, respectively; the limits of quantification of the two methods were 0.13–0.56 and 0.27–1.36 μg/kg and the limits of detection were 0.04–0.23 and 0.08–0.41 μg/kg, respectively. All these figures of merit met the requirements for the determination of quinolones. In order to avoid false positive results, a suitable sample pretreatment method should be chosen for different matrix samples. The two pretreatment methods used in this study, thanks to their ease of operation, high sensitivity and good repeatability, could be suitable for the qualitative and quantitative analysis of multiple veterinary drug residues in porcine tissues.

Key words: EMR-L, Oasis PRiME HLB, liquid-liquid extraction, quinolones, porcine tissues

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