摘要
供试品用无水乙醇超声提取,采用Shim-pack GIST C_(18)-AQ色谱柱分离,以不同体积比的乙腈和0.2%(体积分数)磷酸溶液混合液为流动相梯度洗脱,在波长205 nm下采用高效液相色谱法检测马甲子根、茎、果和叶的化学成分,建立指纹图谱,并同时测定白桦脂酸、白桦脂醛、羽扁豆醇、(+)-γ-生育酚、豆甾醇、维生素E和β-谷甾醇等7种化学成分的含量。采用国家药典委员会发布的中药色谱指纹图谱相似度评价系统(2012版)和SPSS21.0软件评价各部位化学成分的相似度。结果表明,根、茎、果和叶的指纹图谱匹配出54个峰,其中22个为共有峰,并确认了7个共有峰的化学成分。根、茎、叶的化学成分的相似度较大,采样时间差可能使果的化学成分的含量差异较大。7种化学成分的质量浓度在一定范围内与对应的峰面积呈线性关系,检出限(3s/k)为0.01~0.08 mg·L^(-1)。按照标准加入法进行回收试验,回收率为93.3%~108%,测定值的相对标准偏差(n=5)均小于5.0%。方法用于供试品分析,显示7种化学成分在不同部位的含量有一定的差异,其中白桦脂酸的含量最高。
The test sample was ultrasonically extracted with anhydrous ethanol,separated on a Shim-pack GIST C_(18)-AQ column,and eluted using gradient mobile phase composed of acetonitrile and 0.2%(volume fraction)phosphoric acid solution at different volume ratios.The chemical components of the roots,stems,fruits,and leaves of Paliurus ramosissimus were analyzed by high performance liquid chromatography(HPLC)at 205 nm of detection wavelength,and the corresponding chromatography fingerprints were established.The 7 chemical components including betulinic acid,betulinaldehyde,lupeol,(+)-γ-tocopherol,stigmasterol,vitamin E,andβ-sitosterol were determined simultaneously.The similarity of the chemical components in each part was evaluated using the Similarity Evaluation System of Chromatographic Fingerprints of Traditional Chinese Medicine(2012 edition),which issued by the Chinese Pharmacopoeia Committee,and the SPSS 21.0 software.As shown by the results,a total of 54 peaks were matched across the fingerprints of roots,stems,fruits,and leaves,of which 22 were identified as common peaks,and 7 common peaks were assigned to identify chemical components.The chemical components of roots,stems,and leaves exhibited high similarity,whereas the fruit samples showed greater variation,likely due to differences in sampling time.Linear relationships between the corresponding peak areas and mass concentrations of 7 chemical components were kept in definite ranges,with detection limits(3s/k)in the range of 0.01-0.08 mg·L^(-1).Test for recovery was made by the standard addition method,giving results in the range of 93.3%‒108%,with RSDs(n=5)of the determined values less than 5.0%.This method was applied to analysis of the test samples,it was shown that there were distinct differences in the contents of the 7 chemical compounds in plant parts,among which betulinic acid had the highest content.
作者
杨孝容
田怡
张海连
YANG Xiaorong;TIAN Yi;ZHANG Hailian(College of New Energy Materials and Chemistry,Leshan Normal University,Leshan 614000,China;Sichuan Province Key Laboratory of Natural Products and Small Molecule Catalysis,Leshan 614000,China)
出处
《理化检验(化学分册)》
北大核心
2025年第12期1406-1413,共8页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
天然产物化学与小分子催化四川省高校重点实验室项目(No.TRCWYFZCH2019007)
四川省第二批地方普通本科高校应用型示范课程(No.2020-44)
四川省第二批省级一流本科课程(No.2021-979)
四川省2022年省级一流本科课程(No.2022-821)。
关键词
马甲子
高效液相色谱法(HPLC)
化学成分
指纹图谱
相似度评价
Paliurus ramosissimus
high performance liquid chromatography(HPLC)
chemical component
fingerprint
similarity evaluation
