HPLC Determination of Monocrotaline in Crotalaria Sessiliflora by Ultrasonic Extraction Separation
摘 要
采用甲醇超声提取法提取农吉利中农吉利甲素,用高效液相色谱法(HPLC)测定农吉利甲素的含量.用L9(34)正交试验设计优化了提取溶剂、提取温度、提取时间、料液比等试验条件;以甲醇-三乙胺(0.5+99.5)混合溶液(pH 7.0)为流动相,对生物碱提取液进行了色谱分离,农吉利甲素质量浓度在1.0~800 mg·L-1范围内呈线性关系,方法的检出限(3S/N)为0.1 mg·L-1,加标回收率试验的结果在97.8%~102.3%之间.
Abstract
Monocrotaline was separated from sample of crotalaria sessiliflora by ultrasonic extraction with methanol.Influential factors of extraction,including the extraction solvents,time and temperature of extraction as well as the ratio of mass of sample to volume of extraction solvent,were studied and optimized by the method of orthogonal design with L9(34) orthogonal layout.In the HPLC determination,UltimateTM C18 (4.6 mm×250 mm,5 μm) column was used as stationary phase and a mixture of methanol and triethylamine-water (0.5+99.5,pH 7.0) solution,mixed in the ratio of 30 to 70,was used as mobile phase.Linear relationship between values of peak area and concentration of monocrotaline was obtained in the range of 1.0-800 mg·L-1.Detection limit (3S/N) found for the method was 0.1 mg·L-1.Recovery was tested by standard addition method and values of recovery found were ranged from 97.8% to 102.3%.
中图分类号 O657
所属栏目 工作简报
基金项目 广东省社会发展领域科技计划项目(73060)
收稿日期 2008/8/4
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备注樊轻亚(1979-),女,河南南阳人,硕士研究生,研究方向为现代仪器分析在药物分析中的应用.
引用该论文: FAN Qing-ya,FAN Hua-jun,HUANG Xiao-wen,HUANG Yong,QIU Pei-li. HPLC Determination of Monocrotaline in Crotalaria Sessiliflora by Ultrasonic Extraction Separation[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(6): 666~668
樊轻亚,范华均,黄晓文,黄勇,邱佩丽. 超声提取-高效液相色谱法测定农吉利中农吉利甲素[J]. 理化检验-化学分册, 2009, 45(6): 666~668
被引情况:
【1】樊轻亚,游国叶, "聚焦微波辅助提取-酸性染料分光光度法测定农吉利中总生物碱",理化检验-化学分册 51, 289-292(2015)
【2】樊轻亚,许卫军,王万好, "液相色谱-串联质谱法测定农吉利中的黄酮类化合物",理化检验-化学分册 51, 1023-1027(2015)
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参考文献
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【2】ABDUL MUN I M,OSAMU Negishi,TETSUO Ozawa.Antioxidative compounds from crotalaria sessiliflora[J].Biosci Biotechnol Biochem,2003,67(2):410-414.
【3】靖永谦,李宏善,陈瑞华.农吉利中氨基酸成分的研究[J].中药通报,1987,12(7):41-43.
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