摘要
目的采用高效液相色谱-电喷雾三重四极杆质谱法(LC-ESI-MS/MS)测定藤珠胃康颗粒中的9种皂苷类化合物(人参皂苷Re、人参皂苷Rb1、人参皂苷Ro、人参皂苷Rd、人参皂苷Rg1、人参皂苷F2、人参皂苷Rf、姜状三七皂苷R1、竹节参皂苷Ⅳa)。方法采用Hypersil GOLD C18色谱柱(100 mm×2. 1 mm,5μm),流动相为乙腈(A)-0. 02%甲酸水溶液(B),梯度洗脱,柱温30℃,流速0. 8 m L·min^-1,电喷雾离子源(ESI)负离子检测,多反应监测模式(MRM)定量。结果人参皂苷Re、人参皂苷Rb1、人参皂苷Ro、人参皂苷Rd、人参皂苷Rg1、人参皂苷F2、人参皂苷Rf、姜状三七皂苷R1、竹节参皂苷Ⅳa等9种皂苷类化合物的线性范围分别为0. 06~6. 40、0. 18~8. 80、0. 34~33. 60、0. 40~10. 00、0. 53~13. 20、0. 02~3. 84、0. 56~28. 00、3. 76~75. 20、0. 72~14. 40μg·m L^-1,线性关系良好,平均加样回收率为95. 98%~109. 57%,RSD为1. 45%~3. 99%。结论所用方法简便、快速、准确、灵敏度高,可用于藤珠胃康颗粒中多种皂苷类化合物的分析测定。
OBJECTIVE To simultaneously determine 9 ginsenoside compounds from Tengzhu Weikang granules by LC-ESI-MS/MS method. METHODS Hypersil LD C18 column( 100 mm × 2. 1 mm,5 μm) was used for the separation. The mobile phase consisted of A( CH3 CN) and B( 0. 02% formic acid) with gradient elution. The flow rate was 0. 8 m L·min^-1 and the column temperature was set at 30 ℃. For the quantification of ginsenosides,the multiple reaction monitoring( MRM) mode of the mass spectrometer was applied and ESI-MS analysis was monitored in negative mode. RESULTS By using the optimized method,the linearity ranges of 9 analytes were 0. 06-6. 40 μg·m L^-1 ginsenoside Re,0. 18-8. 80 μg·m L^-1 ginsenoside Rb1,0. 34-33. 60 μg·m L^-1 ginsenoside Ro,0. 40-10. 00 μg·m L^-1 ginsenoside Rd,0. 53-13. 20 μg·m L^-1 ginsenoside Rg1,0. 02-3. 84 μg·m L^-1 ginsenoside F2,0. 56-28. 00 μg·m L^-1 ginsenoside Rf,3. 76-75. 20 μg·m L^-1 Panax zingiberensis saponins R1,and 0. 72-14. 40 μg·m L^-1 chikusetsusaponin Ⅳa,respectively. The recoveries of 9 nsenosides in the samples were95. 98%-109. 57% with relative standard deviation( RSD) in the range of 1. 45% to 3. 99%. CONCLUSION The proposed LC-MS/MS method is accurate and reproducible,showing high sensitivity,rapidness,and recovery. This method allows the assessment of various ginsenosides in a single analytical run providing an innovative tool to control Tengzhu Weikang Granules materials quantification.
作者
王鹏飞
白吉庆
王芳
黎丹
权利娜
王小平
WANG Pengfei;BAI Jiqing;WANG Fang;LI Dan;QUAN Lina;WANG Xiaoping(Shaanxi University of Chinese Medicine,Xianyang,Shaanxi,712046 P.R. China)
出处
《华西药学杂志》
CAS
CSCD
2019年第5期494-497,共4页
West China Journal of Pharmaceutical Sciences
基金
陕西省科技厅资助项目(2012KTCL03-14)
陕西省科技厅中药现代化项目[2009K19-03(2)]
