LC-MS/MS测定白及止血海绵中白及葡甘聚糖的含量  

LC-MS/MS in determination of Bletilla striata glucomannan in Blettila striata hemostatic sponge

作　　者：王巍[1] 夏令强 陈君[1] 张晓洁 

机构地区：[1]解放军455医院药剂科,上海200052 [2]总后丰台综合仓库药材供应站,北京100071

出　　处：《第二军医大学学报》2014年第12期1401-1403,共3页Academic Journal of Second Military Medical University

基　　金：南京军区"十一五"医药卫生科研基金(12MA020)~~

摘　　要：目的建立LC-MS/MS方法测定白及止血海绵中白及葡甘聚糖含量。方法采用Waters X BridgeTM Amide（2.1mm×100mm,3.5μm）;流动相为乙腈∶5mmol/L醋酸铵（内含0.1%甲酸水溶液）=60∶40;流速为0.3mL/min;柱温35℃;进样量10μL。结果 D-甘露糖线性范围为50.0-5 000.0ng/mL（r=0.999 5）,方法学考察表明日内和日间精密度、最低检测限和定量限均符合相关标准,加样回收率为98.4%（n=5）,RSD=1.03%。结论本法操作简单,选择性好,灵敏度高,适用于白及止血海绵中的白及葡甘聚糖的定量分析。Objective To establish a LC-MS/MS system for the determination of Bletilla striata glucomannan in Bletilla striata hemostatic sponge. Methods The Waters X BridgeTM Amide（3. 5 μm, 2. 1 min×100 mm）column was used at 35℃ ; acetonitrile and 5 mmol/L ammonium acetate （containing 0.1% formic acid） （60 ： 40, V/V） were used as the mobile phase at a flow rate of 0.3 mL/min, with the injection volume being 10 μL. Results The linear range for D-mannose was 50.0-5 000.0 ng/mL （r=0. 999 5）. The results of intra-day and inter-day precisions, limit of detection and limit of quantitation were all within the normal ranges. The recovery rate （n=5） was 98.4%, RSD= 1.03%. Conclusion The method in this study is simple, selective and sensitive; it can be used for the quantitative determination and quality control of Bletilla striata glueomannan.

关 键 词：白及葡甘聚糖 液相色谱-串联质谱法 白及 

分 类 号：R286.3[医药卫生—中药学]