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机构地区:[1]中国药科大学现代中药教育部重点实验室,南京210009 [2]中国药科大学分析测试中心,南京210009 [3]浙江大学药学院中药科学与工程学院,杭州310027
出 处:《中国天然药物》2006年第4期287-290,共4页
基 金:国家自然科学基金资助项目(No.30472160)~~
摘 要: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.
关 键 词:黄芪皂苷 定量分析 HPLC-ESI/TOF MSD
分 类 号:TQ460.72[医药卫生—药物分析学]
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