LC-MS/MS法同时测定滇龙胆中4种苯甲酸酯类成分  

Simultaneous determination of four benzoate compounds from Gentiana rigescens Franch. by LC-MS / MS

作　　者：潘俊[1] 潘聿[2] 肖丹[1] 李志敏[1] 王元忠[1] 李晚谊[1] 

机构地区：[1]云南省农业科学院药用植物研究所,云南昆明650205 [2]云南中医学院,云南昆明650500

出　　处：《中成药》2014年第12期2550-2553,共4页Chinese Traditional Patent Medicine

基　　金：云南省科技计划项目(2012AE002)

摘　　要：目的建立LC-MS/MS法同时测定滇龙胆中抗老年痴呆的4种主要成分gentiside A,gentiside J,gentiside B,gentiside K的量。方法使用岛津LC-MS/MS 8030液质联用仪,色谱柱为Shim-pack XR-ODSⅢ（75 mm×2.0 mm,1.6μm）;流动相为甲醇-0.1%甲酸,等度洗脱;离子源为电喷雾电离源（ESI）,采用负离子多反应监测模式。结果Gentiside A,gentiside J,gentiside B,gentiside K分别在39.0-444.4μg/m L、39.0-444.4μg/m L、59.0-444.4μg/m L、26.0-444.4μg/m L范围内线性关系良好,相关系数为0.998 9-0.999 6;所测的滇龙胆根部中,4种苯甲酸酯类成分的含有量分别为0.284、0.358、0.654、0.267 mg/g;加样回收率为98.1%-102.6%,RSD为0.7%-1.7%。结论该方法专属性好、精密度高,可用于滇龙胆中苯甲酸酯类成分的检测。AIM A specific liquid chromatography-ion trap mass spectrometric（ LC-MS / MS） method was developed that allowed simultaneous determination of four components（ gentiside A,gentiside J,gentiside B,gentiside K） of anti-dementia in Gentiana rigescens Franch. METHODS By using the LC-MS / MS method,the four compounds were separated on a Shim-pack XR-ODS Ⅲ column（ 75 mm × 2. 0 mm,1. 6 μm） with a mobile phase consisted of methanol and water containing 0. 1% formic acid with isocratic elution. Electrospray ionization source（ ESI） was applied and operated in negative ionization multiple reaction monitoring model. RESULTS The linear ranges of gentiside A,gentiside J,gentiside B and gentiside K were 39. 0 ~ 444. 4 μg / m L（ r = 0. 999 6）,39. 0 ~444. 4 μg / m L（ r = 0. 999 0）,59. 0 ~ 444. 4 μg / m L（ r = 0. 998 9） and 26. 0 ~ 444. 4 μg / m L（ r = 0. 999 4）,respectively. The contents of four benzoate compounds in the root of Gentiana rigescens Franch,were 0. 284,0. 358,0. 654,0. 267 mg / g,respectively. The recoveries ranged from 98. 1% to 102. 6%,and RSDs were in the range of0. 7% ~ 1. 7%. CONCLUSION The method is specific and precise,and can be used for the determination of benzoate compounds in Gentiana rigescens Franch.

关 键 词：滇龙胆 老年痴呆 苯甲酸酯 LC-MS/MS 

分 类 号：R284.1[医药卫生—中药学]