超高效液相色谱-串联质谱法测定牛羊可食性组织中巴氯芬残留量

Determination of Baclofen Residues in Edible Tissue of Ovine and Bovine with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

关键词:  巴氯芬  直过式固相萃取  牛羊可食性组织  超高效液相色谱-串联质谱  同位素内标法

Key words:  baclofen  direct pass solid phase extraction  edible tissure of ovine and bovine  ultra performance liquid chromatography- triple quadrupole tandem mass  isotope internal standard method

摘要:

建立超高效液相色谱-串联质谱测定牛羊可食性组织中巴氯芬残留量的分析方法。取均质后的动物组织经80%(V/V)乙腈甲酸溶液提取, 加入无水硫酸镁和氯化钠进行脱水和盐析，高速离心分层后合并提取液，取适量乙腈层溶液经prime HLB直过式固相萃取柱净化后，以40 ℃氮气吹干。残渣以15%乙腈甲酸溶液复溶后以反相C18为固定相，0.1%甲酸与0.1%甲酸乙腈为流动相，采用梯度洗脱程序进行分离，以串联质谱进行同位素内标法定性定量分析。巴氯芬在0.5~50 μg/kg范围内线性关系良好(r=0.9994)，方法的最低检出限为0.25 μg/kg, 最低定量限为0.50 μg/kg, 添加回收率在89.09%~109.52%内，批内批间变异系数(CV)小于10%。该方法具有较好的准确度与精密度，适用于牛羊可食性组织中巴氯芬残留量的测定。

Abstract:

To establish a method for determination of baclofen residue in edible tissue of ovine and bovine by ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry. Homogenized tissue samples were extracted with 80%(V/V) acetonitrile formic acid solution, and dehydrated and salted out with anhydrous magnesium sulfate and sodium chloride. After high speed centrifugation and stratification, the upper extract was purified with prime HLB column and dried with nitrogen at 40 ℃. The residue was dissolved with 15% acetonitrile formic acid solution. The dissolved solution was separated by gradient elution procedure with C18 column as the stationary phase, and 0.1% formic acid together with 0.1% formic acid acetonitrile as the mobile phase. Triple quadrupole tandem mass spectrometry was used for qualitative and quantitative analysis with isotope internal method. Baclofen had good linear relationships in the range of 0.5~50 μg/kg(r=0.9994). The limit of detection(LOD) of the method was 0.25 μg/kg and the limit of quantitative(LOQ) was 0.50 μg/kg. The recoveries were between 89.09%~109.52%, the coefficient of variation(CV) within and between batches were both lower than 10%. This method has good accuracy and precision, which is suitable for the determination of baclofen residues in edible tissue of pig and chicken.