| 周瑞雪,杜鹃,史宪海,郭景文.少腹逐瘀丸中松香酸的HPLC-MS检测方法研究[J].中国药事,2017,(10):1192-1198 |
| 少腹逐瘀丸中松香酸的HPLC-MS检测方法研究 |
| On HPLC-MS Method to Determine Abietic Acid in Shaofuzhuyu Pills |
| 投稿时间：2016-05-24 |
| DOI：10.16153/j.1002-7777.2017.10.017 |
| 中文关键词: 少腹逐瘀丸 松香酸 没药 高效液相色谱 质谱 |
| 英文关键词: Shaofuzhuyu pills abietic acid myrrh HPLC HPLC-MS/MS |
| 基金项目:2014年中成药国家抽验品种中掺伪染色物的专项检测研究工作；2014年国家药品监督抽验工作 |
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| 中文摘要: |
| 目的：建立少腹逐瘀丸中添加松香酸的HPLC和HPLC-MS/MS检测法。方法：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，流动相为乙腈-0.1%甲酸水，体积流量0.2 mL·min-1，梯度洗脱。结果：松香酸进样量在0.1582~1.582μg·mL-1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。 |
| 英文摘要: |
| 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 0.2 mL·min-1 under gradient elution. Results: A good linearity of rosin acids was observed within 0.1582-1.582 μg·mL-1 and the average recovery was 99.8% (RSD=0.23%). Conclusion: The established method was simple, rapid, accurate and with good specificity, stability and repeatability, which could meet the requirements for the qualitative and quantitative detection of the abietic acid illegally added in Shaofuzhuyu pills. |
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