HPLC-MS/MS测定花椒及其制品中羟基-α-山椒素

The determination of hydroxyl-α-capsaicin in zanthoxylum and its products by HPLC-MS/MS

建立了液相色谱-串联质谱(HPLC-MS/MS)测定花椒及其制品中羟基-α-山椒素的分析方法。样品经70%甲醇水溶液超声提取2次,每次10 min,以0.1%甲酸水溶液和甲醇为流动相梯度洗脱,经C18色谱柱分离,正离子模式扫描,多重反应监测模式检测。以保留时间和特征离子对(母离子和两个碎片离子)信息比较进行定性,外标法定量。结果表明:在2~500 ng/mL范围内,羟基-α-山椒素的线性回归方程相关系数为0.999;样品添加不同浓度梯度的标准溶液,平均回收率在80.8%~94.4%,相对标准偏差(RSD)在0.8%~4.9%。当样品称取为1 g,定容体积为25 mL时,检出限(LOD)为0.05 mg/kg,定量限(LOQ)为0.1 mg/kg。该方法高效快捷、准确度和精密度满足检测要求,能准确测定羟基-α-山椒素的含量,可为花椒及其制品的质量控制提供参考依据。

An analytical method for the determination of hydroxy-α-capsaicin in Zanthoxylum and its products by liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was established.The samples were ultrasonically extracted twice by 70%methanol aqueous solution for 10 min each time,and eluted with 0.1%formic acid aqueous solution and methanol as mobile phase gradient,and were separated by C18 column,scanned in positive ion mode,and detected in multiplex reaction monitoring mode.Retention time and characteristic ion pair(precursor and two fragment ions)information comparison was qualitative,quantified by external standard.The results showed that in the range of 2~500 ng/mL,the correlation coefficient of the linear regression equation by hydroxy-α-capsaicin was 0.999,and the average recovery rate of the sample was 80.8%~94.4%,and the relative standard deviation(RSD)was 0.8%~4.9%.When the sample was weighed to 1 g and the volume was 25 mL,the limit of detection(LOD)was 0.05 mg/kg and the limit of quantification(LOQ)was 0.1 mg/kg.This method was efficient,fast,accurate and precise to meet the detection requirements,and could accurately determine the content of hydroxy-α-capsaicin.This paper can provide a reference for the quality control of zanthoxylum and its products.