摘要
建立了一种利用反相液相色谱法测定青蒿素原料药中脱氢青蒿素和9-表-青蒿素含量的分析方法。采用紫外检测器于210 nm处进行检测,以C-18柱(Agilent Zobax ODS,150 mm×4.6 mm,5μm)为分析柱,以乙腈和水的混合溶液为流动相,采取梯度洗脱方式(0~10 min,45%乙腈;10~20 min,45%~80%乙腈;20~25 min,80%~45%乙腈;25~35 min,45%乙腈)进行洗脱。在此条件下,青蒿素、脱氢青蒿素和9-表-青蒿素能彼此完全分离。脱氢青蒿素和9-表-青蒿素的浓度分别在4.11~28.76、9.42~65.93μg/m L范围内与峰面积的线性关系良好,相关系数R均大于0.998,检出限(3S/N)分别为2.668 ng和75.34 ng,样品加标回收率均在94%~108%之间。
A reversed-phase high performance liquid chromatography (RP-HPLC) is developed for the determination of artemisitene and 9-epi-artemisinin in artemisinin raw material. The method employs a UV detector at 210 nm by using a C-18 column (Agilent Zobax ODS, 150 mm ~ 4.6 mm, 5 μm). The mobile phase consists of acetonitrile and water with different volume ratios and is controlled by a gradient program, in which 45% acetonitrile is kept for 10 min, followed by a linear 10 min gradient to 80% acetonitrile, a linear 5 min gradient to 45% acetonitrile, and maintaining 45% acetonitrile for 10min to recondition the column. Under above-mentioned conditions, the peaks of artemisinin, artemisitene and 9-epi-artemisinin can be separated each other completely. There are good linear relationships between peak area and concentration in the range of 4.11~28.76μg/mL for artemistene, and in the range of 9.42~65.93 μg/mL for 9-epi-artemisinim, the correlation coefficients (R) are all more than 0.998. The limits of detection ((3S/N)) are 2.668 ng and 75.34 ng, respectively. The recoveries by standard addition method are all in the range of 94%~ 108%.
出处
《湖南文理学院学报(自然科学版)》
CAS
2016年第1期24-28,34,共6页
Journal of Hunan University of Arts and Science(Science and Technology)
基金
湖南省教育厅资助科研项目(14A012)
湖南威嘉生物科技有限公司资助科研项目
关键词
青蒿素
脱氢青蒿素
9-表-青蒿素
高效液相色谱法
artemisinin
artemisitene
9-epi-artemisinin
high performance liquid chromatography(HPLC)