响应面优化QuEChERS结合UHPLC-MS/MS法测定乌鳢肌肉中四环素类抗生素

李丽春; 刘书贵; 林嘉薇; 尹怡; 郑光明; 赵城; 马丽莎; 单奇; 戴晓欣; 魏琳婷; 周豪

doi:10.13386/j.issn1002-0306.2022120266

响应面优化QuEChERS结合UHPLC-MS/MS法测定乌鳢肌肉中四环素类抗生素

Response Surface Optimization of the QuEChERS Combined with UHPLC-MS/MS Method for Determination of Tetracyclines in Muscle of Channa argus

摘要

摘要: 为了评估乌鳢中四环素类药物的残留风险，建立了乌鳢肌肉中4种四环素类药物残留的快速、简单、廉价、高效、耐用和安全的前处理方法（Quick、Easy、Cheap、Effective、Rugged、Safe，QuEChER）。采用Box–Behnken design（BBD）响应面优化法，优化了提取和净化条件。样品经10 mL 1%甲酸酸化乙腈和2 mL 0.1 mol/L Na₂EDTA-McIlvaine缓冲溶液提取，以150 mg PSA和200 mg C₁₈进行净化，采用超高效液相色谱-串联质谱法（Ultra-high performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS）检测。结果表明，该方法在0.50~100 ng/mL浓度范围内线性良好（r≥0.999），检出限（Limit of Detection，LOD）和定量限（Limit of Quantitation，LOQ）分别为0.25～0.75 μg/kg和0.84～2.00 μg/kg。在乌鳢肌肉中四环素、土霉素、金霉素和多西环素的平均回收率在89.5%~1187%之间，相对标准偏差（RSD）在1.11%~8.88%之间。该方法简便、灵敏、准确，可用于乌鳢中四环素含量的快速测定。

Abstract: A quick, easy, cheap, effective, rugged and safe pre-treatment method (QuEChERS) was established to evaluate the risk of tetracycline residues in the muscle of Channa argus. The Box-Behnken design (BBD) response surface optimization method was used to optimize the extraction and purification conditions. The samples were extracted with 10 mL acetonitrile (containing 1% formic acid) and 2 mL 0.1 mol/L Na₂EDTA-Mcllvaine buffer solution, and the extracts were purified by 150 mg primary secondary amine（PSA）and 200 mg C₁₈, and detected with Ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The result showed that the calibration curve was linear in the range of 0.50~100 ng/mL, with high correlation coefficients (r≥0.999). The limits of detection (LOD) and quantification (LOQ) were 0.25～0.75 μg/kg and 0.84～2.00 μg/kg, respectively. The average recoveries of tetracycline, oxytetracycline, chlortetracycline and doxycycline at three different spiked levels in the muscle of Channa argus were 89.5%～118%, with relative standard deviations (RSDs) of 1.11%～8.88%. This method is simple, sensitive and accurate, and can be used for the rapid quantitative determination of tetracyclines in Channa argus.

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