固相萃取-液相色谱串联质谱测定饲料中的α-茄碱和α-卡茄碱

Determination ofα-Solanine and α-Carconine in Feed by Solid Phase Extraction-Liquid Chromatography Tandem Mass Spectrometry

建立一种以固相萃取法提取,用高效液相色谱-串联质谱法对饲料中α-茄碱和α-卡茄碱进行定性、定量检测的方法。本实验将饲料样品经10%乙酸水提取后用C_(18)固相萃取柱净化提取,洗脱液用初始流动相定容;再经液相色谱串联质谱上机测定。实验数据显示:线性系数达到0.999以上,加标回收率为89.0%~109.3%,精密度(RSD)为3.96%~5.09%,α-茄碱和α-卡茄碱仪器检出限可达到0.012 mg/kg、0.0048 mg/kg。结果表明,该方法提取回收率高、准确度和精密度高,因此该方法可推广应用至其他相似饲料类型样品。

Established a solid phase extraction method to extractα[WT5BZ]-solanine andα-caconine,and using liquid chromatography-tandem mass spectrometry(LC-MS/MS)for qualitative identification of LC-MS/MS.In this experiment,the feed sample was extracted with 10%acetic acid water and then purified and extracted with a C_(18) solid phase extraction column.The eluent was fixed to volume with the initial mobile phase;then it was measured by liquid chromatography tandem mass spectrometry.The experimental data shows that the linear coefficient is above 0.999,the recovery rate of spiked standard is 89.0%~109.3%,the precision(RSD)is 3.96%~5.09%,and the detection limit ofα-solanine andα-caconine can reach 0.012 mg/kg and 0.0048 mg/kg.The results show that this method has high extraction recovery rate,high accuracy and precision,so this method can be popularized and applied to other samples of similar feed types.