RP-HPLC对不同北细辛商品药材中3种非挥发性成分的含量同时测定及指纹图谱的比较研究  

Simultaneous Quantification of 3 Non-volatile Components and Fingerprints Comparison of Asarum heterotropoides Commercial Herbs Using RP-HPLC

作　　者：温晓茵[1] 吴昊 颜鹏 沈水容 钟山[1] 刘晓东[1,3] 赖克方 WEN Xiao-yin;WU Hao;YAN Peng;SHEN Shui-rong;ZHONG Shan;LIU Xiao-dong;LAI Ke-fang(State Key laboratory of Respiratory Disease,National Clinical Research Center for Respiratory Disease,Guangzhou Institute of Respiratory Health,the First Affiliated Hospital of Guangzhou Medical University^Guangzhou 510182,China;Guangdong Institute of Nanshan Pharmaceutical Innovation,Guangzhou 510530,China;Duke Global Health Institute,Duke Medical Center,Duke University,Durham,North Carolina,27708,the United States)

机构地区：[1]广州医科大学附属第一医院,广州呼吸健康研究院,呼吸疾病国家重点实验室,国家呼吸系统疾病临床医学研究中心,广州510182 [2]广东省南山医药创新研究院,广州510530 [3]杜克大学,杜克医学中心,杜克全球健康研究所,达勒姆,北卡罗来纳州,美国27708

出　　处：《中国药学杂志》2021年第7期578-583,共6页Chinese Pharmaceutical Journal

基　　金：国家自然科学基金项目资助(81503235);广东省自然科学基金项目资助(2019A1515011930,2015A030310309);广东省高校青年创新人才项目资助(2015KQNCX129);广东省中医药局面上项目资助(20171183);广州市科技计划项目资助(201607010355);广州医科大学学术骨干培育计划及慢性咳嗽创新团队项目资助(2017-210,2017-159)。

摘　　要：目的建立不同北细辛商品药材中细辛脂素、芝麻脂素、卡枯醇3种非挥发性成分的含量同时测定方法及指纹图谱,为其质量标准和质量控制优化提供参考。方法 21份北细辛商品药材以体积分数70%乙醇加热回流提取,采用Agilent SB-C_(18)色谱柱(4.6 mm×250 mm, 5μm),以乙腈-水为流动相梯度洗脱,检测波长285 nm,体积流速1.0 mL·min^(-1),柱温30℃,对北细辛非挥发性部位进行同时含量测定、指纹图谱和聚类分析。结果 21份北细辛商品药材中,非挥发性成分细辛脂素含量0.630 6~3.123 3 mg·g^(-1),芝麻脂素含量0.255 4~1.236 8 mg·g^(-1)、卡枯醇含量0.071 4~0.469 4 mg·g^(-1);各样品中非挥发性部位指纹图谱的相似度均在0.989以上;共有成分聚类分析发现大部分批次间差异较小。结论建立非挥发性部位的指纹图谱技术结合多指标同时含量测定方法可为北细辛非挥发性组分科学全面的综合评价方法提供参考。OBJECTIVE To establish the simultaneous quantification method of 3 non-volatile components and fingerprints comparison of Asarum heterotropoides and provide a scientific method for the quality standards and quality control of A.heterotropoides.METHODS Twenty-one batches of A.heterotropoides were extracted by heating and refluxing with 70%ethanol and analyzed by HPLC on Agilent SB-C18 column(4.6 mm×250 mm,5μm),with the mobile phase consisted of acetonitrile and aqueous with a gradient elution for simultaneous quantification of 3 non-volatile components,fingerprints comparison and Cluster analysis.The flow rate was 1.0 mL·min^(-1),the column temperature maintained at 30℃,and the detection wavelengths were set at 285 nm.RESULTS Asarinin,sesamin,and kakuol showed good linearity(r=0.9999)in the ranges of 0.015625-0.5 mg·mL^(-1),0.015625-0.5 mg·mL^(-1) and 0.00625-0.2 mg·mL^(-1),respectively.The average recoveries were 98.31%,97.12%and 95.54%,with RSD 1.59%,1.73%and 2.46%,respectively.The contents of the 3 non-volatile components in the 21 batches of samples were in a range of 0.6306-3.1233 mg·g^(-1) for asarinin,0.2554-1.2368 mg·g^(-1) for sesamin,and 0.0714-0.4694 mg·g^(-1) for kakuol.The similarity coefficient of the fingerprints of 21 batches samples were above 0.989.CONCLUSION There are certain differences in the content of 3 non-volatile components in different batches of A.heterotropoides samples,but the content of asarinin,as the index component of A.heterotropoides,meets the requirements of the Chinese Pharmacopoeia.The established simultaneous quantification method and fingerprints are highly sensitive with strong specificity and it can be used efficiently in the quality control of A.heterotropoides.

关 键 词：北细辛 细辛脂素 芝麻脂素 卡枯醇 非挥发性成分 指纹图谱 

分 类 号：R284[医药卫生—中药学]