HPLC-MS法测定步长脑心通中多种黄芪皂苷类成分

Determination of Eight Astragalosides in BuChang Naoxintong Capsule by HPLC-MS

目的：应用高效液相色谱．电喷雾飞行时间质谱联用（HPLC-ESI／TOF MS）法定量分析步长脑心通胶囊中黄芪皂苷类成分。方法：采用人参皂苷Rgl作为内标物；色谱柱：Zorbax Extend C18，250mm×4、6mm，5μm；柱温25℃；流动相：0．1％甲酸水溶液（A）-乙腈（B），梯度洗脱；流速：1mL·min^-1；质谱采集模式：正离子。结果：各黄芪皂苷的检测限为0．10～0．22ng，定量限为0．22～0．52ng；在对应的线性范围内，r≥0．9982；峰面积之比（Ax／Ai）的日间精密度（RSO）和日内精密度（PSD）均小于2．86％；回收率失于94．9％。结论：本文建立HPLC-ESI／TOF MS法可以准确测定黄芪类中药制剂中的黄芪皂苷类成分。

AIM： To apply high performance liquid chromatography coupled with electrospray ionization time-of-flight mass spectrometry （HPLC-ESI/TOF MS） for quantitative analysis of astragalosides in BuChang Naoxintong Capsule. METHOD： Ginsenoside Rgl was used as internal standard. The chromatographic conditions were as follows： Zorbax Extend C18（250 mm× 4.6mm, 5μm） column; column temperature： 25 ℃; mobile phase： 0.1% formic acid-water （A） and acetonitrile （B）, gradient elute; flow rate： 1 mL · min^-1. Use the ESI source and acquire the data in positive mode. RESULT： The limits of detection （LODs） and limits of quantification （LOQs） of eight astragalnsides were in the range of 0. 10 - 0.22 ng and 0.22～ 0.52ng, respectively. All calibration curves showed good linear regression （r≥0.9982） within test range. The overall intra-, inter-day precision and recovery were less than 2.86% for peak area ratio （As/Ai） and higher than 94.9%, respectively. CONCLUSION： The developed method proved to be suitable for accurate determination of astragalosides in preparations of Traditional Chinese Medicine.