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Inertsil ODS-3,流动相为乙腈-水(梯度洗脱),检测波长为210 nm(党参炔苷)、220 nm(苍术内酯Ⅱ、苍术内酯Ⅲ、丁香苷)、276 nm(苍术内酯Ⅰ),流速为0.8 mL/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(24 h)、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。
OBJECTIVE:To establish a method for simultaneous determination of the contents of codonopatin,syringin,atractylenolideⅠ,atractylenolideⅡand atractylenolideⅢ,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,atractylenolideⅡ,atractylenolideⅢ),276 nm(atractylenolideⅠ).The column temperature was set at 30℃,and the sample size was 20μL.RESULTS:The linear range of codonopatin,syringin,atractylenolideⅠ,atractylenolideⅡand atractylenolideⅢwere 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);the limits of quantification were 2.4460,0.1680,0.2481,0.0657,0.0998μg/mL,and detection limits were 1.3520,0.0672,0.0054,0.0063,0.0073μg/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=6),96.83%-104.16%(RSD=2.62%,n=6),97.87%-100.99%(RSD=1.07%,n=6).The average contents were 33.78-431.82,0-20.60,0.44-3.68,0-10.83,0.27-73.40μg/g.The content of 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. 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 ofatractylenolide Ⅱ in C. pilosula was higher than C. pilosula Nannf. var. modesta(Nannf.)L. T. Shen,but was no detected in C.tangshen
作者
刘付松
陈翠莎
孙佩
刘莎
韦中兰
刘小琪
吴发明
LIU Fusong;CHEN Cuisha;SUN Pei;LIU Sha;WEI Zhonglan;LIU Xiaoqi;WU Faming(College of Pharmacy,Zunyi Medical University,Guizhou Zunyi 563003,China;Industrial Crop Research Institute,Sichuan Academy of Agriculture Sciences,Chengdu 610300,China)
出处
《中国药房》
CAS
北大核心
2020年第14期1677-1682,共6页
China Pharmacy
基金
国家自然科学基金资助项目(No.81760679)
国家重点实验室开放课题(No.FAMP201808K)
贵州省教育厅青年科技人才成长项目(No.黔教合KY字〔2017〕196)
遵义医学院大学生创新创业训练计划(No.遵医201751087)。
