超高效液相色谱-串联质谱法测定猪肉中巴氯芬的残留

Determination of baclofen in meat by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法测定猪肉中巴氯芬残留量的方法。方法样品采用0.1 moL/L盐酸-甲醇溶液(20:80,V:V)提取,混合型强阳离子交换柱(MCX)净化,经C18反相色谱柱分离后,正离子扫描,多反应监测模式检测巴氯芬,基质标曲定量。结果该方法在1~500 ng/mL浓度范围内线性良好,r2=1,检出限为1μg/kg,定量限为5μg/kg,回收率为75.28%~77.86%,精密度RSD<10%。结论该方法灵敏度高、特异性强,适用于猪肉中巴氯芬残留量的分析。

Objective To establish a method for the determination of baclofen in meat by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was extracted by hydrochloride methanol, purified by solid-phase extraction cartridges (MCX) and separated on a reversed phase. Using ESI+ with multiple reactions monitoring (MRM), identification of baclofen residue was performed and quantified by matrix extracted calibration curve. Results Calibration curve was linear between 1 and 500 ng/mL with the correlation coefficient of 1. The limit of detection was 1 μg/kg and the limit of quantitation was 5 μg/kg. The recoveries were 75.28%-77.86%, and relative standard deviations (RSDs) were less than 10%. Conclusion This method has high sensitivity and high specificity, which is suitable for the determination of the baclofen residual amount in meat.