HPLC法同时测定蒙药达乌里芯芭中梓醇和益母草苷的含量
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摘要
目的:建立同时测定蒙药达乌里芯芭中梓醇和益母草苷含量的方法。方法:采用高效液相色谱法。色谱柱为XSelect HSS T3 C18,流动相为乙腈-1.0%磷酸水溶液(梯度洗脱),流速为1 m L/min,柱温为40℃,检测波长为203 nm,进样量为10μL。采用建立的方法测定7批达乌里芯芭样品中梓醇和益母草苷的含量。结果:梓醇、益母草苷进样量检测线性范围分别为0.17~3.4、0.25~5.0μg(r均≥0.999 5),检测限分别为3.57、4.72 ng,定量限分别为12.24、41.98 ng,精密度、稳定性(24 h)、重复性试验的RSD均<2.0%(n=6),加样回收率分别为93.0%~97.3%、92.1%~97.9%(RSD分别为1.9%、2.4%,n=6)。7批样品中梓醇、益母草苷的含量分别为0.53~0.81、0.79~1.25 mg/g。结论:建立的方法快速简便、稳定可靠,可用于达乌里芯芭中梓醇和益母草苷含量的同时测定。
OBJECTIVE:To develop a method for simultaneous determination of catalpol and leonuride in Mongolian medicine Cymbaria dahurica. METHODS:HPLC method was adopted. The determination was performed on XSelect HSS T3 C18 column with mobile phase consisted of acetonitrile-1.0% phosphoric acid water solution(gradient elution) at the flow rate of 1 m L/min.The column temperature was set at 40 ℃,and the detection wavelength was set at 203 nm. The sample size was 10 μL. Established method was adopted to determine the contents of catalpol and leonuride in 7 batches of C. dahurica samples. RESULTS:The linear range of catalpol and leonuride were 0.17-3.4 and 0.25-5.0 μ g(r≥0.999 5). The detection limits were 3.57 and 4.72 ng,respectively. The quantitative limits were 12.24 and 41.98 ng,respectively. RSDs of precision,stability(24 h)and reproducibility tests were all lower than 2.0%(n=6). The average recoveries were 93.0%-97.3%(RSD=1.9%,n=6) and 92.1%-97.9%(RSD=2.4%,n=6). The contents of catalpol and leonuride in 7 batches of samples were 0.53-0.81 and 0.79-1.25 mg/g,respectively. CONCLUSIONS:The established method is rapid,simple,stable and reliable,and can be used for simultaneous determination of catalpol and leonuride in C. dahurica.
OBJECTIVE:To develop a method for simultaneous determination of catalpol and leonuride in Mongolian medicine Cymbaria dahurica. METHODS:HPLC method was adopted. The determination was performed on XSelect HSS T3 C18 column with mobile phase consisted of acetonitrile-1.0% phosphoric acid water solution(gradient elution) at the flow rate of 1 m L/min.The column temperature was set at 40 ℃,and the detection wavelength was set at 203 nm. The sample size was 10 μL. Established method was adopted to determine the contents of catalpol and leonuride in 7 batches of C. dahurica samples. RESULTS:The linear range of catalpol and leonuride were 0.17-3.4 and 0.25-5.0 μ g(r≥0.999 5). The detection limits were 3.57 and 4.72 ng,respectively. The quantitative limits were 12.24 and 41.98 ng,respectively. RSDs of precision,stability(24 h)and reproducibility tests were all lower than 2.0%(n=6). The average recoveries were 93.0%-97.3%(RSD=1.9%,n=6) and 92.1%-97.9%(RSD=2.4%,n=6). The contents of catalpol and leonuride in 7 batches of samples were 0.53-0.81 and 0.79-1.25 mg/g,respectively. CONCLUSIONS:The established method is rapid,simple,stable and reliable,and can be used for simultaneous determination of catalpol and leonuride in C. dahurica.
引文
[1]国家中医药管理局《中华本草》编辑委员会.中华本草:蒙药卷[M].上海:上海科学技术出版社,2004:219.
[2]国家药典委员会.中华人民共和国卫生部药品标准:蒙药分册[S].北京:中国医药科技出版社,1998:18.
[3]包银苹,王青虎,代那音台.蒙药芯芭中2个环烯醚萜苷的结构鉴定[J].内蒙古民族大学学报(自然科学版),2017,32(5):446-448.
[4]LI ZH,LONG P,BAI S,et al.Chemical constituents from Cymbaria dahurica L.(Scrophulariaceae)[J].Biochemical Systematic&Ecology,2014,57(7):11-14.
[5]扈颖慧.蒙药达乌里芯芭根部化学成分的研究[D].呼和浩特:内蒙古大学,2015.
[6]SZIGETI J,TóTH L,BUJTáS G,et al.Chemical study of Cymbaria dahurica L.[J].Acta Pharm Hung,1981,51(2):72-85.
[7]王鸿宇.达乌里芯芭茎部化学成分的研究[D].呼和浩特:内蒙古大学,2015.
[8]卫冰,杨云.地黄环烯醚萜苷类化学成分的研究进展[J].中国中医药现代远程教育,2011,19(24):130-133.
[9]国家药典委员会.中华人民共和国药典:一部[S].2015年版.北京:中国医药科技出版社,2015:124-125.
[10]董炤,陈长勋.梓醇药理作用研究进展[J].中成药,2013,35(5):1047-1051.
[11]张振涛,吴仁奇,张威,等.芯芭的抗氧化作用及对肾缺血再灌注损伤的保护作用[J].内蒙古医科大学学报,2003,25(1):1-3.
[12]戴静秋.西北风毛菊、蒙古芯芭、丝毛飞廉3种药用植物化学成分和生物活性的研究[D].兰州:兰州大学,2002.
[13]李旻辉,常燕琴,张春红.蒙药芯芭正丁醇提取物在制备防治糖尿病药物中的应用:中国,104352624A[P].2015-02-18.
[14]国家药典委员会.中华人民共和国药典:四部[S].2015年版.北京:中国医药科技出版社,2015:375.
[15]邬国栋,张佳,白露,等.高效液相色谱法测定蒙药芯芭中梓醇的含量[J].包头医学院学报,2013,6(5):13-15.
[16]LIAO QF,JIA Y,GAO QT,et al.High-performance liquid chromatographic method for determination and pharmacokinetic study of chlorogenic acid in the plasma of rats after administration of the Chinese medicinal preparation Luying decoction[J].Chromatographia,2007,2(2):166-172.
[17]荚丽丽,魏岚,赵健,等.了哥王药材中7种成分的含量测定及其主成分、聚类分析[J].中国药房,2017,28(33):4706-4710.
[2]国家药典委员会.中华人民共和国卫生部药品标准:蒙药分册[S].北京:中国医药科技出版社,1998:18.
[3]包银苹,王青虎,代那音台.蒙药芯芭中2个环烯醚萜苷的结构鉴定[J].内蒙古民族大学学报(自然科学版),2017,32(5):446-448.
[4]LI ZH,LONG P,BAI S,et al.Chemical constituents from Cymbaria dahurica L.(Scrophulariaceae)[J].Biochemical Systematic&Ecology,2014,57(7):11-14.
[5]扈颖慧.蒙药达乌里芯芭根部化学成分的研究[D].呼和浩特:内蒙古大学,2015.
[6]SZIGETI J,TóTH L,BUJTáS G,et al.Chemical study of Cymbaria dahurica L.[J].Acta Pharm Hung,1981,51(2):72-85.
[7]王鸿宇.达乌里芯芭茎部化学成分的研究[D].呼和浩特:内蒙古大学,2015.
[8]卫冰,杨云.地黄环烯醚萜苷类化学成分的研究进展[J].中国中医药现代远程教育,2011,19(24):130-133.
[9]国家药典委员会.中华人民共和国药典:一部[S].2015年版.北京:中国医药科技出版社,2015:124-125.
[10]董炤,陈长勋.梓醇药理作用研究进展[J].中成药,2013,35(5):1047-1051.
[11]张振涛,吴仁奇,张威,等.芯芭的抗氧化作用及对肾缺血再灌注损伤的保护作用[J].内蒙古医科大学学报,2003,25(1):1-3.
[12]戴静秋.西北风毛菊、蒙古芯芭、丝毛飞廉3种药用植物化学成分和生物活性的研究[D].兰州:兰州大学,2002.
[13]李旻辉,常燕琴,张春红.蒙药芯芭正丁醇提取物在制备防治糖尿病药物中的应用:中国,104352624A[P].2015-02-18.
[14]国家药典委员会.中华人民共和国药典:四部[S].2015年版.北京:中国医药科技出版社,2015:375.
[15]邬国栋,张佳,白露,等.高效液相色谱法测定蒙药芯芭中梓醇的含量[J].包头医学院学报,2013,6(5):13-15.
[16]LIAO QF,JIA Y,GAO QT,et al.High-performance liquid chromatographic method for determination and pharmacokinetic study of chlorogenic acid in the plasma of rats after administration of the Chinese medicinal preparation Luying decoction[J].Chromatographia,2007,2(2):166-172.
[17]荚丽丽,魏岚,赵健,等.了哥王药材中7种成分的含量测定及其主成分、聚类分析[J].中国药房,2017,28(33):4706-4710.