高效液相色谱-串联质谱法测定鸡蛋中地克珠利、妥曲珠利及其代谢物残留量

Determination of diclazuril, toltrazuril and its two metabolites in eggs by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  QuEchERs  高效液相色谱-串联质谱法  鸡蛋  地克珠利  妥曲珠利

英文关键词:QuEchERs  high performance liquid chromatography-tandem mass spectrometry  eggs  diclazuril  toltrazuril

中文摘要:

      摘 要: 目的 建立高效液相色谱-串联质谱法测定鸡蛋中地克珠利和妥曲珠利及其代谢物残留量的方法。方法 样品经0.1%甲酸乙腈提取, 提取液用50 mg N-丙基乙二胺(primary secondary amine, PSA)粉末、50 mg C18粉末和150 mg无水硫酸镁进行净化, 以5 mmol/L 乙酸铵-乙腈作为流动相进行梯度洗脱, 采用电喷雾负离子模式扫描, 多反应监测(multiple reaction monitoring, MRN)技术进行定性分析, 内标法定量。结果 地克珠利和妥曲珠利及其代谢物在2~50 ng/mL线性范围内线性关系良好, 相关系数均大于0.99; 检出限为0.2~3.0 μg/kg, 定量限为0.3~6.0 μg/kg; 在加标回收试验中的回收率范围为80.4%~117.9%, 相对标准偏差(relative standard deviations, RSDs, n=5)为1.0%~4.8%。采用该方法对市售的20批次鸡蛋样品进行检测, 未在样品中检出地克珠利和妥曲珠利及其代谢物, 同时做质控样品, 回收率等指标符合分析要求。结论 该方法具有快速、选择性好、重现性好等优点, 有效提高了检测质量和效率, 降低了检测成本, 并且易于实现批量化操作; 为抗球虫药物残留检测、风险评估提供了科学依据。

英文摘要:

      ABSTRACT: Objective To establish method for the determination of diczulide and toltrazuril and their metabolites in eggs by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted by 0.1% formic acid acetonitrile solution and the extraction solution was purified using 50 mg primary secondary amine (PSA) powder, 50 mg C18 powder, and 150 mg anhydrous magnesium sulfate. then gradient eluted with 5 mmoL/L ammonium acetate-acetonitrile as mobile phase, and scanned by electrospray negative ion mode. Multiple reaction monitoring (MRN) was used for qualitative analysis and internal standard method for quantitative analysis. Results The linear relationship between diczulil and toltrazuril and their metabolites was good in the linear range of 2–50 ng/mL, and the correlation coefficients were greater than 0.99. The limits of detection and quantitation were 0.2–3.0 μg/kg and 0.3–6.0 μg/kg respectively. The recoveries ranged from 80.4% to 117.9% and the relative standard deviations (RSDs) was 1.0% to 4.8%. The method was used to detect 20 batches of egg samples in the market, diclazuriland toltrazuril and its two metabolites were not detected in the samples. At the same time, quality control samples were taken, and the recovery rate and other indicators met the analysis requirements. Conclusion This method has the advantages of being fast, selective, and reproducible. Meanwhile, the detection cost is reduced, and mass operation can be easy achieved. These results provide scientific basis for detection and risk assessment of coccidiostats residues.