| 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(2.1 mm×100 mm, 3.5 μm);流动相为乙腈:5 mmol/L醋酸铵(内含0.1%甲酸水溶液)=60:40;流速为0.3 mL/min;柱温35℃;进样量10 μL。结果 D-甘露糖线性范围为50.0～5 000.0 ng/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。 |
| 关键词: 白及葡甘聚糖 液相色谱-串联质谱法 白及 |
| DOI：10.3724/SP.J.1008.2014.01401 |
| 投稿时间：2014-04-11修订日期：2014-05-27 |
| 基金项目:南京军区“十一五”医药卫生科研基金(12MA020). |
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| LC-MS/MS in determination of Bletilla striata glucomannan in Blettila striata hemostatic sponge |
| WANG Wei1,XIA Ling-qiang1,CHEN Jun1,ZHANG Xiao-jie2* |
(1. Department of Pharmacy, No. 455 Hospital of PLA, Shanghai 200052, China;
2. Medical Supply Station, Fengtai Warehouse of PLA General Logistics Department, Beijing 100071, China
*Corresponding author) |
| Abstract: |
| 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 mm×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 glucomannan. |
| Key words: Bletilla striata glucomannan liquid chromatography-mass spectrometry Blettila |
