固相萃取-液相色谱串联质谱法测定猪尿中的巴氯芬

Determination of Baclofen in Pig Urine by High-Performance Liquid Chromatograph-Tandem Mass Spectrometry

关键词:  巴氯芬  猪尿  液相色谱-串联质谱法  残留

Key words:  baclofen  pig urine  LC-MS/MS  residue

摘要:

为了建立用固相萃取-液相色谱串联质谱法测定动物尿液中巴氯芬药物残留的检测方法，试验采用叔丁醇-叔丁基甲醚对猪尿样品进行提取，提取液经混合型阳离子固相萃取小柱（MCX）净化、富集后，以液相色谱串联质谱测定，外标法定量。结果表明，该方法检出限为0.2 ng/mL，定量限为0.8 ng/mL，巴氯芬在0.8~20 ng/mL的添加浓度范围内线性良好，线性相关系数大于0.9997，在低、中、高（0.8、1.6、5.0 ng/mL）三个浓度的添加水平回收率在80%~120%之间，批内、批间精密度均小于10%。该方法灵敏度高，定性、定量准确，可用于猪尿中巴氯芬药物残留的定性、定量检测。

Abstract:

A simple and sensitive LC-MS/MS method for determination of baclofen in pig urine was developed. The sample was extracted by the mixture of tert-butanol and tert-butyl methyl ether, and purified by MCX cartridges. The analyte was determined by LC-MS/MS with extermal standard for quantification. The limit of detection and limit of quantity were found to be 0.2 ng/mL and 0.8 ng/mL, respectively. The standard curve of baclofen within the range of 0.8 to 20 ng/mL was in good linearity, the correlation coefficients were greater than 0.9995, the recoveries ranged from 80% to 120%(0.8,1.6,5.0 ng/mL), and intra- and inter-batch variation coefficients were lower than 10% for low, middle and high concentrations.