少腹逐瘀丸中松香酸的HPLC－MS检测方法研究-中国药事.PDFVIP

1192 ·技术研究 · 少腹逐瘀丸中松香酸的HPLC-MS检测方法研究 * 周瑞雪，杜鹃，史宪海，郭景文 （山西省食品药品检验所，太原 030001） 摘要 目的： 方法： 建立少腹逐瘀丸中添加松香酸的 HPLC 和 HPLC-MS/MS 检测法。 采用 HPLC、 HPLC-PDA、HPLC-MS 等。色谱柱为 C18 柱（250 mm×4.6 mm，5μm），体积流量 1.0 mL·min-1 ， 流动相为乙腈 -0.1% 甲酸水（82 ∶ 18），检测波长为 241 nm。液质联用验证采用 C18 柱，流动相为乙 -1 结果： -1 腈 -0.1% 甲酸水，体积流量 0.2 mL·min ，梯度洗脱。 松香酸进样量在 0.1582 ～ 1.582μg·mL 与峰面积呈良好的线性关系；平均加样回收率为 99.8%，RSD 为 0.23%。结论：该方法简便、快速、准 确，专属性稳定性及重复性均良好。本文所建立的检测方法，可满足定性定量检测少腹逐瘀丸中非法添 加松香酸的要求。 关键词： 少腹逐瘀丸；松香酸；没药；高效液相色谱；质谱 R927.1 A 1002-7777(2017)10-1192-07 中图分类号： 文献标识码： 文章编号： doi:10.16153/j.1002-7777.2017.10.017 On HPLC-MS Method to Determine Abietic Acid in Shaofuzhuyu Pills * Zhou Ruixue, Du Juan, Shi Xianhai, Guo Jingwen (Shanxi Provincial Institute for Food and Drug Control, Taiyuan 030001, China) Abstract Objective: To establish HPLC and HPLC-MS/MS methods to determine abietic acid added in Shaofuzhuyu pills. Methods: HPLC, HPLC-PDA, HPLC-MS, etc were used. A C18 column (250 mm×4.6 mm, 5μm) was adopted for the determination. The mobile phase was composed of acetonitrile and 0.1% formic acid (82 ∶18) at a flow rate of 1.0 mL min-1. The detection wavelength was 241 nm. The verification of LC-MS was · carried out on a C18 column. Mobile phase was composed of acetonitrile and 0.1% formic acid at a flow rate of -1 0.2 mL min under gradient elution. Results: A good linearity of rosin acids was observed within 0.1582-1.582 · -1 μg mL and the average recovery was 99.8% (RSD=0.23%). Conclusion: The established method was simple, · rapid, accurate and