摘要
目的 :用LC MS/MS法测定中药吴茱萸、黄柏、白鲜及其制剂中吴茱萸内酯的含量。方法 :分析柱 :DiscoveryC1 8,1 50mm× 2 .1mm ;预柱 :SymmetryC1 8;柱温 2 0℃。流动相 :A :水 - 0 .1 %醋酸 ;流动相B :乙腈 - 0 .1 %醋酸 ;梯度洗脱 ;流速 :0 .2mL·min- 1 。检测通道 1 (1S) 1 87.0 >1 30 .9;检测通道 2 (吴茱萸内酯 ) 4 71 .7>1 61 .2供试品用甲醇—氯仿 (1∶3)提取 ,与适量内标溶液 (补骨脂素 )混合后进样分析。结果 :吴茱萸内酯在 2 5～ 1 0 0 0ng·mL- 1 浓度范围内呈良好的线形关系 ,其回归方程为C =3 .1 2 4As/Ai- 1 .935× 1 0 - 3,r =0 .9996 ;样品的平均加样回收率 1 0 0 .2 %。结论 :本法的检测灵敏度高、专属性强 ,样品预处理简便。
Objective: To develop a simple LC MS/MS method for the measurement of limonin in fructus evodiae, cortex phellodendri, cortex dictamni and its preparation. Methods: Separation was obtained by using a discovery C 18 column (150mm×2.1 mm), The mobile phase:A:water-0.1%HAc;B:acetonitrile-0.1%HAc;The elution program was gradient and the flow rate was 0.2mL·min -1 . The mass detector was set MS1(IS)=187.0 and MS2(Limonin)=471.0 by multiple reaction monitor(MRM) respectively.The sample was added psoralen(IS), then extracted with methanol chloroform(1∶3).Results: Limonin was linear from 25 to 1000ng·mL -1 ( r = 0.9996), The regression equation was C=3.124 As/Ai 1.935×10 -3 . The average recovery was 100.2%.Conclusion: This method is simple, quick, sensitive and exclusive.
出处
《中成药》
CAS
CSCD
北大核心
2003年第2期144-146,共3页
Chinese Traditional Patent Medicine
基金
上海市徐汇区卫生局科研基金 (编号C0 1一 58)
