【摘要】 建立了超高压液相色谱-串联质谱（UHPLC-MS/MS）法同时测定牛奶粉中常见抗吸虫药物（氯氰碘柳胺、硝碘酚腈、碘醚柳胺和三氯苯达唑）残留的方法。样品中药物残留经乙腈提取、Captiva EMR-Lipid固相萃取柱净化、Waters CORTECS UPLC C18色谱柱（50 mm×3.0 mm, 1.6μm）分离，在电喷雾离子源负离子多反应监测模式（Multiple reaction monitoring, MRM）下采用质谱测定，外标法定量。本方法检测抗吸虫药物残留的线性浓度范围为1.0～100.0μg/L，相关系数（r）均大于0.997，方法的检出限为0.58～1.10μg/kg，定量限为2.61～4.95μg/kg。在5.0、50.0和80.0μg/kg的空白基质加标水平下，平均回收率为93.2%～105.3%，日间相对标准偏差（Inter-relative standard deviations, Inter-RSDs）为2.8%～9.3%。本方法具有通量高、灵敏准确和精密度好等优点，可用于奶粉中抗吸虫药物的日常检测和监控监测。更多还原

【Abstract】 A method for determination of common fasciolicide(Closantel, nitroxinil, rafoxanide, triclabendazole and ketotriclabnedazole) residues in milk powder using ultra-high pressure liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS) was developed. The samples were extracted with acetonitrile, and then cleaned-up with Captiva EMR-Lipid solid phase extraction column. The liquid chromatographic separation was carried out on a Waters CORTECS UPLC C18 column by a gradient elution with 5 mmol/L ammonium acetate solution-acetonitrile as mobile phases. Mass spectrometric analysis was conducted by multi-reaction monitoring(MRM) in electrospray negative ionization mode. The quantitative analysis was carried out by matrix-matched standard curve withr>0.997in the concentration ranges of fasciolicide residues within 1.0–100.0μg/L. The limits of detection(LOD) and limits of quantification(LOQ) of this method were 0.58–1.10μg/kg and 2.61–4.95μg/kg, respectively. The recoveries of the spiked samples at three levels(5.0, 50.0 and 80.0μg/kg) ranged from 93.2% to 105.3% with the relative standard deviations(RSDs) from 1.2% to 8.9%, and the inter-RSDs were in the range of 2.8%–9.3%. The proposed approach, characterizing with high throughput and sensitivity, good accuracy and precision as well, could be effectively applicable to determination of fasciolicide residues in milk powder in routine detection as well as surveillance analysis.更多还原