色谱 ›› 2018, Vol. 36 ›› Issue (11): 1119-1131.DOI: 10.3724/SP.J.1123.2018.06007

• 研究论文 • 上一篇    下一篇

QuEChERS-超高效液相色谱-串联质谱法测定鸡蛋中125种兽药残留

方从容1, 高洁1, 王雨昕1, 周爽1, 赵云峰1, 陈达炜1, 郭启雷2   

  1. 1. 国家食品安全风险评估中心, 卫生部食品安全风险评估重点实验室, 北京 100021;
    2. 安捷伦科技有限公司, 北京 100102
  • 收稿日期:2018-06-12 出版日期:2018-11-08 发布日期:2014-09-30
  • 通讯作者: 陈达炜.Tel:(010)67779768,E-mail:dila2006@163.com.
  • 基金资助:

    国家自然科学基金青-科学基金项目(21607035).

Determination of 125 veterinary drugs residues in eggs by QuEChERS-ultra-high performance liquid chromatography-tandem mass spectrometry

FANG Congrong1, GAO Jie1, WANG Yuxin1, ZHOU Shuang1, ZHAO Yunfeng1, CHEN Dawei1, GUO Qilei2   

  1. 1. China National Centre for Food Safety Risk Assessment, Key Laboratory of Food Safety Risk Assessment, Ministry of Health, Beijing 100021, China;
    2. Agilent Technologies, Beijing 100102, China
  • Received:2018-06-12 Online:2018-11-08 Published:2014-09-30
  • Supported by:

    National Natural Science Foundation of China (No. 21607035).

摘要:

采用冷冻脂质过滤,结合分散固相萃取净化的QuEChERS方法,建立了超高效液相色谱-串联质谱法测定鸡蛋中125种兽药残留的检测方法。样品中的11类兽药(硝基咪唑类、苯并咪唑类、磺胺类、喹诺酮类、四环素类、大环内酯类、雄激素类、孕激素类、糖皮质醇类、雌激素类、氯霉素类)用70%(v/v)乙腈-水溶液(含0.1 mol/L EDTA)提取后,提取液在-20℃冷冻处理2 h,再经分散固相萃取法净化,净化液经稀释后,以超高效液相色谱-串联质谱法测定,外标法定量。结果显示125种兽药的线性相关系数R2≥0.99,定量限范围为2.0~60 μg/kg,回收率在60.4%~119.3%之间,相对标准偏差在0.3%~16.1%之间。该方法前处理简单、准确、成本较低,适用于鸡蛋中兽药残留的高通量快速检测分析。

关键词: QuEChERS, 超高效液相色谱-串联质谱, 鸡蛋, 兽药

Abstract:

To establish a method for the determination of veterinary drug residues in eggs by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), samples were extracted and purified using frozen lipid filtration combined with the QuEChERS method taking advantage of dispersive solid-phase extraction (DSPE). A total of 125 veterinary drug residues in eggs were analyzed, encompassing 11 classes of drugs (nitroimidazoles, benzimidazoles, sulfonamides, quinolones, macrolides, tetracyclines, androgens, progestational hormones, glucocorticoids, estrogens, and chloramphenicols). The drugs were extracted in acetonitrile/water (70:30, v/v) containing 0.1 mol/L EDTA. The precipitation of lipids and proteins was promoted by performing the extractions at very low temperature (-20℃) for 2 h. Further purification was carried out using dispersive solid-phase extraction (DSPE) followed by dilution of the supernatant. Detection and analysis of veterinary drug residues by UHPLC-MS/MS was conducted and quantified by the external standard method. Our results showed that this method gave good linearity within a certain concentration range (relative coefficient, R2 ≥ 0.99), and the acceptable limits of quantification were determined to be 2.0-60 μg/kg for the 125 veterinary drugs. Good recovery values (60.4%-119.3%) were achieved for all the 125 veterinary drugs with RSD values ranging from 0.3% to 16.1%. This method proved suitable for the rapid determination of veterinary drug residues in eggs with a simple, accurate, and low-cost procedure.

Key words: egg, QuEChERS, ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), veterinary drugs

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