液相色谱-质谱法测定鸡肉中四环素残留的2种定量方法比较

Comparison of Two Quantitative Methods for the Determination of Tetracycline Residues in Chicken by Liquid Chromatography-Mass Spectrometry

为比较液相色谱-质谱/质谱不同的定量处理方法对鸡肉中四环素检测结果的影响,以Na2EDTA-Mcllvainc缓冲液提取样品,经HLB固相萃取柱净化,使用液相色谱-串联质谱法测定,采用2种不同定量方法对鸡肉中四环素进行定量分析。结果表明,在10~500 ng/mL线性范围内,R2≥0.997,检出限为10μg/kg,在25,50和250μg/kg 3个添加水平和能力验证样品测试下,使用溶剂工作曲线定量的阴性鸡肉样品加标回收率为40.2%~72.8%,能力验证样品四环素z值分别是-3.42和-3.38,使用基质工作曲线法定量的阴性鸡肉样品加标回收率为85.1%~107%,能力验证样品z值分别是0.80和0.85。基质工作曲线法的四环素检测结果准确性显著高于优于溶剂工作曲线法,可为四环素的检测分析提供参考。

To compare the effects of different quantification methods using liquid chromatography-tandem mass spectrometry(LC-MS/MS)on the detection of tetracycline in chicken meat,the samples were extracted with Na2 EDTA-Mcllvainc buffer,purified with HLB solid-phase extraction columns,and analyzed using LC-MS/MS.Two different quantification methods were employed for the analysis of tetracycline in chicken meat.The results showed that within the linear range of 10-500 ng/mL,R2≥0.997,and the limit of detection was 10μg/kg.At the spiking levels of 25,50,and 250μg/kg,the recovery rates of spiked negative chicken meat samples quantified using the solvent calibration curve method ranged from 40.2%to 72.8%,with z-values for proficiency testing samples being-3.42 and-3.38,respectively.In contrast,using the matrix calibration curve method,the recovery rates for spiked negative chicken meat samples ranged from 85.1%to 107%,with z-values for proficiency testing samples being 0.80 and 0.85.The accuracy of tetracycline detection using the matrix calibration curve method was significantly higher than that of the solvent calibration curve method,providing a valuable reference for tetracycline analysis.