高效液相色谱-串联质谱法测定羌活中异欧前胡素和紫花前胡苷

目的：建立高效液相色谱-串联质谱法测定羌活中异欧前胡素和紫花前胡苷含量。方法：羌活样品超声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%乙酸水溶液和乙腈，梯度洗脱。串联质谱在多反应监测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：异欧前胡素和紫花前胡苷的检出限分别为0.03 ng·mL^-1和0.015 ng·mL^-1，定量限分别为0.10 ng·mL^-1和0.05 ng·mL^-1，异欧前胡素和紫花前胡苷平均回收率分别为93.6%和94.5%，RSD分别为2.4%和2.6%。结论：该方法经方法学验证，可用于羌活中异欧前胡素和紫花前胡苷的分析。

Objective: To establish a high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for the determination of isoimperatorin and nodakenin in Notopterygium incisum. Methods: The sample was extracted by ultraphonic extraction,and diluted in methanol for further analysis.The analysis was performed on a C₁₈ column(150 mm×2.1 mm,3.5 μm)using a gradient elution program with the mobile phase of 0.1% acetic acid solution and acetonitrile.The analyte was determined by an electrospray ionization tandem mass spectrometry in multiple reactions monitoring(MRMs)mode.The qualitative and quantitative analyses were 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 isoimperatorin and nodakenin were 0.03 ng·mL^-1 and 0.015 ng·mL^-1,and the limits of quantification(LOQs)were 0.10 ng·mL^-1 and 0.05 ng·mL^-1.The average recovery was 93.6% with RSD of 2.4% for isoimperatorin,94.5% with RSD of 2.6% for nodakenin. Conclusion: This established method is simple,reliable,and sensitive,which is suitable for the analysis of isoimperatorin and nodakenin in Notopterygium incisum.