羊肉中多黏菌素A和多黏菌素B液相色谱-串联质谱检测方法的建立

Development of a Liquid Chromatography-tandem Mass Spectrometry(LC-MS/MS)Method for Detection of Colistin A and Colistin B in Mutton

[目的]建立一种液相色谱-串联质谱同步测定羊肉中多黏菌素A和多黏菌素B的方法。[方法]样品经10%三氯乙酸水溶液-乙腈溶液提取,WCX固相萃取柱净化,0.1%甲酸水溶液作为流动相进行梯度洗脱,流速0.30 mL/min,多反应监测(MRM)正离子模式扫描,用液相色谱-串联质谱仪检测,基质添加标准溶液外标法定量。[结果]多黏菌素A和多黏菌素B在5.0~110.0μg/L浓度范围内呈良好线性关系,线性相关系数R>0.996,方法的定量限为0.50μg/kg,3个添加水平的平均回收率为73.2%~115.6%,RSD≤10.0%。[结论]该方法高效、准确,适用于羊肉样品中多黏菌素A和多黏菌素B的定量及确证检测。

[Objective]To develop a liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for simultaneous detection of colistin A and colistin B in mutton.[Method]The samples were extracted with 10%trichloroacetic acid aqueous solution-acetonitrile solution,and then the targets were purified and enriched with WCX solid phase extraction column.The targets were gradiently eluted using 0.1%formic acid aqueous solution as mobile phase with a flow rate of 0.3 mL/min.After screening by multiple reaction monitoring(MRM)under positive ion mode,the targets were detected by LC-MS/MS and were quantitatively determined by external standard method with addition of standard solution in matrix.[Result]Colistin A and colistin B had a good linear relationship in the range of 5.0-110.0μg/L,and the linear correlation coefficients were above 0.996.The limit of quantitation of the developed LC-MS/MS method was 0.50μg/kg.At three adding levels,the average recoveries ranged from 73.2%to 115.6%with relative standard deviations(RSD)≤10.0%.[Conclusion]The developed LC-MS/MS method is highly efficient and accurate,and is applicable for quantitative and confirmatory determination of colistin A and colistin B in mutton samples.