液相色谱-质谱法测定茜草中芦西丁含量-中国中医药信息杂志.PDF

·96· Chinese Journal of Information on TCM Dec.2016 Vol.23 No.12 液相色谱-质谱法测定茜草中芦西丁含量 浦益琼，丁越，王冰，张若曦，张彤 上海中医药大学，上海 201203 摘要：目的 运用液相色谱-质谱法测定茜草药材中芦西丁的含量。方法 采用 Agilent 1290HPLC-G6460 三重四级杆质谱仪，在 ESI- 离子模式下选择离子监测，色谱分离采用Agilent Eclipse Plus C18 RRHD 色谱柱 （2.1 mm ×50 mm，1.8 µm ），以0.1% 甲酸- 乙腈（70 ∶30 ）为流动相，柱温30 ℃，流速0.4 mL/min ，进样量 2 µL。结果 芦西丁在 0.005 2 ～2.64 ng 范围内呈良好线性关系（r ＝0.999 9 ），80%、100%、120%浓度水平的 加样回收率为 94.80% ～100.94% （平均97.17% ，RSD ＝6.16% ），方法重复性及精密度均良好。结论 本研究 建立的方法灵敏、准确，重复性好，适用于茜草中芦西丁的含量测定，可用于茜草药材中该成分的限度检查。 关键词：茜草；芦西丁；液相色谱-质谱联用 DOI：10.3969/j.issn.1005-5304.2016.12.023 中图分类号：R284.1 文献标识码：A 文章编号：1005-5304(2016)12-0096-03 Content Determination of Lucidin in Rubiae Radix et Rhizoma by LC-MS PU Yi-qiong, DING Yue, WANG Bing, ZHANG Ruo-xi, ZHANG Tong (Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China) Abstract: Objective To develop a LC-MS method for the content determination of lucidin in Rubiae Radix et Rhizoma. Methods Agilent 1290 HPLC and G6460 Mass were used for quantification in MRM mode under ESI-. chromatography was performed on a Agilent Eclipse Plus C18 RRHD column (2.1 mm × 50 mm, 1.8 µm) at 30 ℃ using acetonitrile-0.1% formic acid in water at the flow rate of 0.4 mL/min. The injection volume was 2 µL. Results Good linearity was obtained from concentration of lucidin among the range of 0.005 2–2.64 ng (r= 0.999 9). Recoveries at different concentrations (80%, 100%, 120%) were between 94.80% and 100.94% (AVE=97.17%, RSD=6.16%). Good reproducibility and precision were also achieved. Conclusion The new developed LC-MS method is sensitive, accurate and with good repeatability, which is suitable for the c