摘要
目的：建立快速灵敏的超高效液相色谱-串联质谱检测注射用双黄连粉针剂中7种活性成分（绿原酸、咖啡酸、芦丁、木犀草苷、连翘酯苷A、黄芩苷、连翘苷）含量的方法.方法：采用Agilent Zorbax C18色谱柱（2.1 mm×50 mm,1.7 μm）,流动相乙腈-0.1％甲酸,梯度洗脱,体积流量0.40 mL· min^-1,柱温30℃.质谱条件为电喷雾离子（ESI）源,负离子模式检测,多重反应监测（MRM）扫描,定量离子对为m/z 353.0 ～ 191.1（绿原酸）,m/z 179.1 ～ 135.1（咖啡酸）,m/z609.2～300.2（芦丁）,m/z447.1 ～285.1（木犀草苷）,m/z 623.1～ 161.1（连翘酯苷A）,m/z 444.8 ～ 268.8（黄芩苷）,m/z 578.8 ～ 370.8（连翘苷）.结果：7个成分在考察的线性范围内,进样浓度与峰面积之间线性关系良好（r＞0.998 3）,精密度RSD＜4.2％;重复性RSD＜6.3％,平均加样回收率在92.2％ ～102.7％.结论：该方法准确、快速、重复性好,可为双黄连粉针剂的质量控制提供参考方法.
Objective： To establish a quick and sensitive UPLC-MS-MS method for simultaneously determining seven components （chlorogenic acid, caffeic acid, rutin,, galuteolin, forsythoside A, baiealin and forsythin） in Shuanghuanglian powder injection. Method： The analysis was performed on an Agilent Zorhax C18 column （2. 1 mm ×50 mm, 1.7 μm） using acetonitrile-0. 1% formic acid as mobile phase, with a gradient elution at the flow rate of 0.40 mL ·min^-1. The column temperature was maintained at 30 ℃. Then the processed sample was analyzed by tandem mass spectrometer with negative electrospray ionization （ESI） source, monitored under a multiple reaction monitoring （MRM） mode, using the transition m/z 353.0 -191. 1, m/z 179.1 - 135. 1, m/z 609.2- 300.2, m/z 447.1 - 285.1, m/z 623.1 - 161.1, m/z 444.8 - 268.8, m/z 578.8 - 370.8 for chlorogenic acid, caffeic acid, turin, galuteolin, forsythoside A, baicalin, forsythin, respectively. Result： The calibration curves were linear in certain ranges for seven compounds （r 〉 0. 998 3） respectively, all the RSDs of precision were less than 4.2% , and all the RSDs of repeatability were less than 6.3%. The average recovery ranged from 92.2% to 102.7%. Conclusion： This method is rapid, accurate, and suitable for the quality control of Shuanghuanglian injection powder.
出处
《中国实验方剂学杂志》
CAS
北大核心
2014年第13期80-84,共5页
Chinese Journal of Experimental Traditional Medical Formulae
基金
国家级大学生创新创业训练计划项目(201313705006)
四川省教育厅理科重点项目(12ZA026)
成都医学院综合性设计性实验项目(ZH201209)
