高效液相色谱-串联质谱测定香辛料中的去甲乌药碱

Determination of Higenamine in Spices by High Performance Liquid Thromatography-Tandem Mass Spectrometry

建立了高效液相色谱-串联质谱(HPLC-MS/MS)快速测定香辛料中去甲乌药碱的分析方法。实验优化了样品前处理条件和色谱质谱条件。在优化条件下,样品经体积比为80%甲醇-水提取,纯水进行一定倍数的稀释,以Waters XBridge C18(150 mm×2.1mm,5μm)色谱柱分离,电喷雾正离子扫描,多反应监测(MRM)模式检测,基质匹配标准溶液外标法定量,实现了香辛料中去甲乌药碱的精确定量分析。去甲乌药碱在0.05~20.0 ng/mL范围内线性关系良好,相关系数为0.9999,方法检出限为0.7μg/kg,定量限为2.33μg/kg,在3个添加水平条件下八角的平均回收率为91.80%~99.97%,相对标准偏差为1.43%~2.35%。该方法简单、灵敏、准确性高、稳定性好,适用于香辛料中去甲乌药碱的测定。

A rapid analytical method for determination of higenamine in spices had been developed by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) in this work. The sample pretreatment conditions and the HPLC-MS/MS conditions were optimized. The sample was extracted with 80% methanol water by volume, and then diluted with pure water for a certain number of times. The target compound was separated on a Waters XBridge C18(150 mm×2.1 mm, 5 μm) column, and determined using electrospray ionization(ESI) source in positive mode with the multiple reaction monitoring(MRM) acquisition mode. It was quantified with the matrix-matched external standard method, which was performed to accurately quantify higenamine in spices. The results showed that this method exhibited a good linearity in the range of 0.05~20.0 ng/mL, with the correlation coefficients(r) of 0.9999. The limit of detetion(LOD, S/N=3) were 0.7 μg/kg, and the limit of quantitation(LOQ, S/N=10) were 2.33 μg/kg. At the three spiked levels, the average recoveries of star anise were in the range of 91.80%~99.97% with the relative standard deviations of 1.43%~2.35%. The method is simple, sensitive, accurate, stable and suitable for the rapid determination of higenamine in spices.