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

作　　者：周瑞雪 杜鹃 史宪海 郭景文 

机构地区：[1]山西省食品药品检验所,太原030001

出　　处：《中国药事》2017年第10期1192-1198,共7页Chinese Pharmaceutical Affairs

基　　金：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

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 m L·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 m L·min-1,梯度洗脱。结果:松香酸进样量在0.1582~1.582μg·m L-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。Objective To establish HPLC and HPLC-MS/MS methods to determine abietic acid added inShaofuzhuyu pills. Methods： HPLC, HPLC-PDA, HPLC-MS, etc were used. A C18 column （250 mmx4.6 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 · min1. The detection wavelength was 241 nm. The verification of LC-MS wascarried out on a C18 column. Mobile phase was composed of acetonitrile and 0.1% formic acid at a flow rate of0.2 mL · min1 under gradient elution. Results： A good linearity of rosin acids was observed within 0.1582-1.582gg · mL1 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 thequalitative and quantitative detection of the abietic acid illegally added in Shaofuzhuyu pills.

关 键 词：少腹逐瘀丸 松香酸 没药 高效液相色谱 质谱 

分 类 号：R927.1[医药卫生—药学]