不同品种及采收期党参药材中5种有效成分含量的比较研究
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篇名: 不同品种及采收期党参药材中5种有效成分含量的比较研究
TITLE: Comparative Study on Contents of 5 Active Ingredients in Different Varieties and Harvesting Periods of Codo- nopsis Radix
摘要: 目的:建立同时测定党参药材中党参炔苷、丁香苷、苍术内酯Ⅰ、苍术内酯Ⅱ和苍术内酯Ⅲ含量的方法,并比较不同品种及采收期党参药材中上述5种成分的含量。方法:采用高效液相色谱法(HPLC)。色谱柱为InertsilODS-3,流动相为乙腈-水(梯度洗脱),检测波长为210nm(党参炔苷)、220nm(苍术内酯Ⅱ、苍术内酯Ⅲ、丁香苷)、276nm(苍术内酯Ⅰ),流速为0.8mL/min,柱温为30℃,进样量为20μL。结果:党参炔苷、丁香苷、苍术内酯Ⅰ、苍术内酯Ⅱ和苍术内酯Ⅲ检测质量浓度的线性范围为44.30~886.00μg/mL(r=0.9997)、6.50~130.03μg/mL(r=0.9996)、4.47~89.46μg/mL(r=0.9995)、2.53~50.50μg/mL(r=0.9994)、5.64~112.80μg/mL(r=0.9995);定量限分别为2.4460、0.1680、0.2481、0.0657、0.0998μg/mL,检测限分别为1.3520、0.0672、0.0054、0.0063、0.0073μg/mL;精密度、稳定性(24h)、重复性、耐用性试验的RSD均小于2%;加样回收率分别为98.87%~100.62%(RSD=0.73%,n=6)、98.46%~101.54%(RSD=1.15%,n=6)、98.32%~101.12%(RSD=1.19%,n=6)、96.83%~104.16%(RSD=2.62%,n=6)、97.87%~100.99%(RSD=1.07%,n=6)。含量分别为33.78~431.82、0~20.60、0.44~3.68、0~10.83、0.27~73.40μg/g。党参炔苷含量由高到低为党参>川党参>素花党参>洛党参;丁香苷为党参>素花党参>川党参,在洛党参中未检出;苍术内酯Ⅰ为素花党参>洛党参>党参>川党参;苍术内酯Ⅱ为党参>素花党参,在川党参和洛党参中未检出;苍术内酯Ⅲ为党参>素花党参>洛党参>川党参。6~10月采收的党参药材中均以党参炔苷含量最高;6~10月苍术内酯Ⅰ含量均较低;8月苍术内酯Ⅱ未检出;9月苍术内酯Ⅰ、苍术内酯Ⅱ含量较低,且丁香苷、苍术内酯Ⅱ在部分样品中未检出。结论:所建HPLC法操作简单、准确、灵敏度高、重复性好,可用于同时测定党参药材中5种有效成分的含量;不同品种及采收期党参药材中5种有效成分含量存在较大差异。
ABSTRACT: OBJECTIVE:To establish a method for simultaneous determination of the contents of codonopatin ,syringin, atractylenolide Ⅰ,atractylenolide Ⅱ and atractylenolide Ⅲ,and to compare the contents of above 5 components in different varieties and harvesting periods of Codonopsis Radix. METHODS :HPLC method was used. The column was Inertsil ODS- 3 with mobile phase consisted of acetonitrile-water (gradient elution )at the flow rate of 0.8 mL/min. The detection wavelengths were 210 nm (codonopatin),220 nm (syringin,atractylenolide Ⅱ ,atractylenolide Ⅲ),276 nm (atractylenolide Ⅰ). The column temperature was set at 30 ℃ ,and the sample size was 20 μ L. RESULTS:The linear range of codonopatin ,syringin, atractylenolide Ⅰ,atractylenolide Ⅱ and atractylenolide Ⅲ were 44.30-886.00 μg/mL(r=0.999 7),6.50-130.03 μg/mL(r=0.999 6), 4.47-89.46 μg/mL(r=0.999 5),2.53-50.50 μg/mL(r=0.999 4),5.64-112.80 μg/mL(r=0.999 5);the limits of quantification were 2.446 0,0.168 0,0.248 1,0.065 7,0.099 8 μg/mL,and detection limits were 1.352 0,0.067 2,0.005 4,0.006 3,0.007 3 μ g/mL;RSDs of precision ,stability(24 h),repeatability and durability tests were all less than 2%;the recoveries were 98.87%-100.62%(RSD=0.73%,n=6),98.46%-101.54% (RSD=1.15%,n=6),98.32%-101.12%(RSD=1.19%,n= 96.83%-104.16%(RSD=2.62%,n=6),97.87%-100.99% (RSD=1.07%,n=6). The average contents were 33.78-431.82, 0-20.60,0.44-3.68,0-10.83,0.27-73.40 μ g/g. The content of 1271985629@qq.com codonopatin was in descending order was as follows as Codonopsis pilosula >C. tangshen >C. pilosula Nannf. var. modesta (Nannf.) L. T. Shen >ecotypic variety of C.·1677· tangshen. The content of syringin in descending order was C. pilosula >C. pilosula Nannf. var. modesta(Nannf.)L. T. Shen >C. tangshen,but it was not detected in ecotypic variety of C. tangshen . The content of atractylenolide Ⅰ in descending order was C. pilosula Nannf. var. modesta(Namf.)L. T. Shen >ecotypic variety of C. tangshen >C. pilosula >C. tangshen . The content of atractylenolide Ⅱ in C. pilosula was higher than C. pilosula Nannf. var. modesta(Nannf.)L. T. Shen ,but was no detected in C. tangshen and ecotypic variety of C. tangshen . The content of atractylenolide Ⅲ in descending order was C. pilosula >C. pilosula Nannf. var. modesta(Nannf.)L. T. Shen >ecotypic variety of C. tangshen >C. tangshen . In Codonopsis Radix collected from Jul. to Oct. ,the content of codonopatin was the highest ;the content of atractylenolide Ⅰ was lower in sample collected from Jun. to Oct.;atractylenolide Ⅱ was not detected in sample collected in Aug. ;the contents of atractylenolide Ⅰ and atractylenolide Ⅱ were the lower in sample collected in Sept. ,and syringin and atractylenolide Ⅱ were not detected in some samples. CONCLUSIONS : The established HPLC method is simple ,accurate,highly sensitive and reproducible. It can be used to simultaneously determine 5 active ingredients contents of Codonopsis Radix ;there are great difference in contents of 5 active ingredients in different varieties and harvesting periods of Codonopsis Radix.
期刊: 2020年第31卷第14期
作者: 刘付松,陈翠莎,孙佩,刘莎,韦中兰,刘小琪,吴发明
AUTHORS: LIU Fusong ,CHEN Cuisha ,SUN Pei,LIU Sha,WEI Zhonglan ,LIU Xiaoqi ,WU Faming
关键字: 党参;党参炔苷;丁香苷;苍术内酯Ⅰ;苍术内酯Ⅱ;苍术内酯Ⅲ;高效液相色谱法;品种;采收期;含量测定
KEYWORDS: Codonopsis Radix ;Codonopatin;Syringin;Atractylenolide Ⅰ;Atractylenolide Ⅱ;Atractylenolide Ⅲ;HPLC;
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