高效液相色谱-串联质谱法测定马铃薯中的α-茄碱和α-卡茄碱

Determination ofα-Solanine andα-Chaconine in Potatoes by HPLC-MS/MS

建立高效液相色谱-串联质谱分析方法测定马铃薯中的α-茄碱和α-卡茄碱。样品经0.5%甲酸-乙腈提取后,盐析分层,经C18固相萃取剂净化。使用Xbridge BEH C_(18)色谱柱分离,采用电喷雾电离源正离子模式进行电离,多反应监测模式采集进行定性定量。α-茄碱和α-卡茄碱的基质标准曲线在10.0~1000μg·L^(-1)范围内线性良好,相关系数R^(2)分别为0.9996和0.9994,3水平加标回收实验中,平均回收率在85.7%~99.5%,相对标准偏差为1.89%~3.31%,方法检出限(LOD)均为0.1 mg·kg^(-1),定量限均为0.3 mg·kg^(-1)。该方法操作便捷,分离效果好,回收率、灵敏度、重现性均能满足日常样品的分析要求。

Analytical method of determination forα-solanine andα-chaconine in potatoes by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was established.After extracted by 0.5%formic acidacetonitrile,analytes were salted out with acetonitrile and the supernatant was purified by C18 solid phase extractant.Finally,the treatment solution was separated by Xbridge BEH C_(18) chromatographic column and ionized by electrospray ionization source(ESI)with positive ion mode,while the qualitative and quantitative ion pairs were acquired by multi-selected reaction monitoring(MRM)mode.The calibration curves ofα-solanine andα-chaconine exhibited a good linearity in the range of 10.0~1000μg·L^(-1) and the correlation coefficients(R^(2))were 0.9996 and 0.9994,respectively.In the three levels spike recovery experiment,average recoveries ranged from 85.7%~99.5%,while the relative standard deviations were 1.89%~3.31%.The limits of detection(LOD)ofα-solanine andα-chaconine were both 0.1 mg·kg^(-1) and limits of quantitation(LOQ)were both 0.3 mg·kg^(-1).This method is efficient to operate,and the methodological results show that this method has good separation effect.In addition,the recovery rate,sensitivity,and reproducibility could satisfy the analysis requirements of daily samples.