微波辅助萃取-高效液相色谱-串联质谱法测定温郁金中3个姜黄素类化合物

目的:建立微波辅助萃取-高效液相色谱-串联质谱法测定温郁金中姜黄素、去甲氧基姜黄素、双去甲氧基姜黄素的含量。方法:温郁金样品经微波辅助萃取甲醇稀释后分析。色谱分离采用C₁₈反相色谱柱(150 mm×2.1 mm, 3.5 μm), 流动相为0.1%醋酸水溶液和乙腈, 梯度洗脱。串联质谱在多反应监测(MRM)模式下检测目标分析物, 以保留时间和特征离子对(母离子和2个碎片离子)信息比较进行定性和定量分析。结果:上述3个姜黄素类化合物的检出限(LOD)为0.02~0.16 ng·mL^-1, 定量限(LOQ)为0.05~0.53 ng·mL^-1, 姜黄素、去甲氧基姜黄素、双去甲氧基姜黄素平均回收率为94.6%、96.5%、95.3%, RSD分别为2.3%、2.6%、2.2%。结论:该方法简便、准确、灵敏, 可用于温郁金中3个姜黄素类化合物的分析。

Objective:To establish a high performance liquid chromatography-tandemed mass spectrometry(HPLC-MS/MS)method coupled with microwave-assisted extraction for the determination of curcumin,demethoxycurcumin,bisdemethoxycurcumin in Curcuma wenyujin Y.H. Chen et C.Ling.Methods:The sample was extracted by microwave-assisted extraction,diluted with methanol for further analysis.The analysis was performed on a C₁₈ column(150 mm×2.1 mm, 3.5 μm)with a gradient elution program using mobile phase of 0.1% acetic acid and acetonitrile.The analyte was determined by an electrospray ionization tandem mass spectrometry in multiple reactions monitoring(MRMs)mode.The qualitative and quantitative analysis was performed based on the retention times and characteristic ion pairs consisting of one parent ion and two fragment ions of the analyte.Results: The limits of detection(LODs)for 3 curcuminoids were in the range of 0.02-0.16 ng·mL^-1, and the limits of quantification(LOQs)were in the range of 0.05-0.53 ng·mL^-1.The average recoveries were 94.6% with RSD of 2.3% for curcumin,96.5% with RSD of 2.6% for demethoxycurcumin,and 95.3% with RSD of 2.2% for bisdemethoxycurcumin,respectively.Conclusion:This method is simple,reliable,and sensitive,which is suitable for the analysis of three curcuminoids in Curcuma wenyujin Y.H. Chen et C.Ling.