液相色谱—质谱法测定茜草中芦西丁含量
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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 ...
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