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细薄星芒海绵总萜烯的制备及Stellettin B和Stellettin D的含量测定
熊巍,王增蕾,林厚文,李志勇,童耕雷,陈万生
0
(上海交通大学生命科学技术学院,海洋生物技术实验室,上海,200240;第二军医大学长征医院药学部,上海,200003)
摘要:
目的:建立测定细薄星芒海绵Stelletta tenuis Lindgren总萜烯提取物中Stellettin B和D含量的方法.方法:采用HPLC-DAD方法.色谱条件为YMC Pack-SIL分析柱(250 mm×4.6 mm,5 μm);流动相为正己烷:乙酸乙酯(75:25),分析时间30 min,流速1.0 ml·min-1;检测波长:360 nm;柱温:室温;进样量:20μl.结果:线性回归方程为Stellettin B:Y=52 181 633 X+957 495(r=0.996 9),线性范围为2.4~30μg;Stellettin D:Y=62 636 828 X-451 022(r=0.998 0),线性范围为2.0~32μg.精密度、稳定性和重现性试验的RSD在3.07﹪~4.76﹪之间.10批细薄里芒海绵总萜烯中Stellettin B和Stellettm D的平均含量分别为59.93﹪(RSD=4.48﹪)和30.98﹪(RSD=2.97﹪).结论:该法为测定细薄星芒海绵总萜烯中有效成分提供了快速、准确、有效的方法.
关键词:  细薄星芒海绵、总萜烯、色谱法,高效液相
DOI:10.3724/SP.J.1008.2006.00787
投稿时间:2005-10-27修订日期:2006-06-05
基金项目:国家高技术研究发展计划(863计划)(2002AA628160,2004628050);上海市青年科技启明星计划(02QB14003);上海市科委中药现代化专项基金(04DZ19809).
Preparation of total isomalabaricanes and determination of Stelletin B and Stellettin D in Stelletta tenuis Lindgren by high pressure liquid chromatography
XIONG Wei,WANG Zeng-lei,LIN Hou-wen,LI Zhi-yong,TONG Geng-lei,CHEN Wan-sheng
(上海交通大学生命科学技术学院,海洋生物技术实验室,上海,200240;第二军医大学长征医院药学部,上海,200003)
Abstract:
Objective:To establish a method for determining the contents of Stellettin B and Stellettin D in total isomalabaricanes in different batches of Stelletta tenuis Lindgren. Methods: A high pressure liquid chromatography (HPLC) method was applied. The column YMC Pack-SIL (250 mm×4.6 mm, 5 μm) was used at room temperature, and the mobile phase was nhexane : ethyl acetate (75 : 25) with a flow rate at 1.0 ml · min^-1 for 30 min. UV detector wave length was at 360 nm. Resuits: The regression equation were:Y=52 181 633 X+957 495(r=0. 996 9)for Stellettin B and Y=62 636 828 X-451 022 (r=0. 998 0) for Stellettin D,with the linear range being 2.4-30μg and 2.0-32μg, correspondingly. The RSD values for accuracy test, stability test and repeatability test were 3.07%-4.76%. The average contents of Stellettin B and Stellettin D in total isomalabaricanes in different batches of Stelletta tenuis Lindgren were 59. 93% and 30. 98%, respectively. Conclusion: This HPLC method provides a fast, accurate and effective way to determine the active contents in total isomalabaricanes from Stelletta tenuis Lindgren.
Key words:  Stelletta tenuis Lindgren  total isomalabarieanes  chromatography,high pressure liquid