摘要
建立了同时测定抗肿瘤中药复方——重楼消瘤方中重楼皂苷Ⅰ、重楼皂苷Ⅱ、重楼皂苷Ⅶ、柴胡皂苷a、柴胡皂苷d 5种皂苷类成分含量的超高效液相色谱-蒸发光散射检测(UPLC-ELSD)法。复方制剂经甲醇提取,采用Waters Cortecs UPLC C18(150 mm×2.1 mm,1.6μm)色谱柱分离,乙腈-水为流动相进行梯度洗脱,蒸发光散射检测器进行检测,以外标法定量。结果显示,5种皂苷类成分的分离度良好,分别在7.1174~177.94μg/mL、 9.4072~235.18μg/mL、 8.8726~221.82μg/mL、 7.4862~187.15μg/mL、9.761 3~244.03μg/mL范围内线性关系良好,相关系数(r)为0.999 2~0.999 8,检出限为0.7~1.0μg/mL,定量下限为1.8~2.4μg/mL;平均回收率分别为93.9%、103%、102%、104%、105%,相对标准偏差(RSD)分别为3.8%、4.0%、4.2%、3.6%、3.2%。该方法简便、快速、准确,可同时对重楼消瘤方中的5个皂苷类成分进行分析,能有效地消除杂质干扰,为重楼消瘤方的质量评价提供实验依据。
An ultra performance liquid chromatography(UPLC) coupled with evaporative light scattering detection(ELSD) was established for the simultaneous determination of 5 saponins,i. e.polyphyllin I,polyphyllin Ⅱ,polyphyllin Ⅶ,saikosaponin a and saikosaponin d in Chonglou Xiaoliu Formula. The samples were extracted with methanol, then separated on a Waters Cortecs UPLC C18(150 mm × 2. 1 mm,1. 6 μm) column with acetonitrile-water as the mobile phase by gradient elution,finally determined by ELSD and quantified by external standard calibration method.The results showed that there were good linear relationships for 5 saponins in the ranges of 7. 117 4-177. 94 μg/mL,9. 407 2-235. 18 μg/mL,8. 872 6-221. 82 μg/mL,7. 486 2-187. 15 μg/mL and 9. 761 3-244. 03 μg/mL, respectively, with their correlation coefficients(r) of 0. 999 2-0. 999 8.The limits of detection and the limits of quantitation were in the ranges of 0. 7-1. 0 μg/mL and 1. 8-2. 4 μg/mL, respectively. The average recoveries were 93. 9%,103%,102%,104%and 105%,with their relative standard deviations(RSDs) of 3. 8%,4. 0%,4. 2%,3. 6% and 3. 2%,respectively.With the advantages of simplicity,rapidness and accuracy,the method could be applied in simultaneous analysis of 5 saponins in Chonglou Xiaoliu Formula and effective elimination of the impurity interference. And it also provides a reference for the quality evaluation on Chonglou Xiaoliu Formula.
作者
胥爱丽
曹颖男
张素中
邱锦燕
谢灿辉
毕晓黎
肖观林
XU Ai-li;CAO Ying-nan;ZHANG Su-zhong;QIU Jin-yan;XIE Can-hui;BI Xiao-li;XIAO Guan-lin(Guangdong Province Engineering Technology Research Institute of T.C.M,Guangzhou 510095,China;College of Pharmacy,Guangzhou Xinhua University,Guangzhou 510520,China;Guangdong Provincial Key Laboratory of Research and Development in Traditional Chinese Medicine,Guangzhou 510095,China;The Fifth Clinical Medicine School,Guangzhou University of Chinese Medicine,Guangzhou 510405,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第2期221-226,共6页
Journal of Instrumental Analysis
基金
2021年度广东省重点建设学科科研能力提升项目(2021ZDJS143)
2021年省属科研机构稳定性支持项目(粤财科教[2021] 113号)。
关键词
重楼消瘤方
皂苷类成分
超高效液相色谱
蒸发光散射
Chonglou Xiaoliu Formula
saponins
ultra performance liquid chromatography
evaporative light scattering detection
