不同产地锁阳水溶性部位HPLC指纹图谱及含量测定研究  

Study on HPLC Fingerprints and Content Determination of Water Fraction of Cynomorii Herba from Different Producing Areas

作　　者：顾志荣[1] 孙岚萍 钱倩 吴国泰 石磊[1] 许爱霞[1] 葛斌[1] GU Zhirong;SUN Lanping;QIAN Qian;WU Guotai;SHI Lei;XU Aixia;GE Bin(Gansu Provincial People's Hospital,Lanzhou 730000,China;Gansu University of Chinese Medicine,Lanzhou 730000,China;Gansu Province Key Laboratory of Pharmacology and Toxicology of Traditional Chinese Medicine,Lanzhou 730000,China)

机构地区：[1]甘肃省人民医院,甘肃兰州730000 [2]甘肃中医药大学,甘肃兰州730000 [3]甘肃省中药药理与毒理学重点实验室,甘肃兰州730000

出　　处：《中国中医药信息杂志》2020年第11期82-88,共7页Chinese Journal of Information on Traditional Chinese Medicine

基　　金：甘肃省中药药理与毒理学重点实验室开放基金(ZDSYS-KJ-2018-010);甘肃省中药质量与标准研究重点实验室开放基金(ZYZL18-004);甘肃省人民医院研发攻关项目(18GSSY2-3)。

摘　　要：目的建立12个产地锁阳水溶性部位的HPLC指纹图谱、3种成分同时测定及主成分分析(PCA)评价方法。方法采集5个省(区)12个市(区/州/旗)的95批锁阳,提取水溶性部位。采用WondaSil C18-WR色谱柱(4.6 mm×150 mm,5μm),以甲醇-0.1%甲酸水溶液(9∶91)为流动相,流速0.8 mL/min,柱温30℃,检测波长258 nm,进样量10μL,建立HPLC指纹图谱及没食子酸、原儿茶酸、儿茶素含量测定方法。对12个产地锁阳水溶性部位的指纹图谱进行相似度分析,以指纹图谱共有峰峰面积为变量建立PCA模型,进行质量评价与产区鉴别,采用载荷分析寻找不同产区样品共有峰差异。结果12个产地锁阳水溶性部位HPLC指纹图谱的主要色谱峰一致,共指认出16个共有峰,除阿拉善左旗、阿拉善右旗、和田样品外,其余产地样品指纹图谱与对照图谱的相似度均大于0.9。没食子酸、原儿茶酸、儿茶素分别在0.022~0.330、0.002~0.030、0.080~1.200μg范围内线性关系良好,相关系数分别为0.9998、0.9993、0.9994,平均加样回收率分别为100.54%、99.82%、99.62%,RSD分别为1.71%、1.95%、2.07%。锁阳水溶性部位没食子酸、原儿茶酸、儿茶素含量分别为0.0313~7.0316、0.0255~0.3963、0.0035~0.7934 mg/g。PCA可将锁阳样品按12个市级产区、5个省级产区进行质量评价与归类分析,载荷分析筛选出导致不同产地锁阳水溶性部位整体质量差异的5个化学成分。结论本研究建立的分析方法稳定、准确、可靠,可用于不同产地锁阳的综合质量评价及产区鉴别。Objective To establish HPLC fingerprints and simultaneous determination of 3 components and quality evaluation methods of water fraction of Cynomorii Herba from 12 producing areas based on principal component analysis(PCA).Methods Totally 95 batches of Cynomorii Herba from 12 cities in 5 provinces were collected and water fractions were extracted.HPLC fingerprints and simultaneous determination method of gallic acid,protocatechuic acid and catechin were achieved on WondaSil C18-WR column(4.6 mm×150 mm,5μm),with methanol-0.1%formic acid solution(9:91)as mobile phase for gradient elution.The flow rate was 0.8 mL/min;column temperature was 30℃;detection wavelength was 258 nm;injection volume was 10μL.Fingerprints of water fraction of Cynomorii Herba from 12 producing areas were analyzed for similarity.Taking common peak areas of fingerprints as variables,PCA models were established for quality evaluation and identification of different producing areas.Loading analysis was used to find differences in common peaks of samples from different producing areas.Results The main peaks of HPLC fingerprints of water fraction of Cynomorii Herba from 12 producing areas were consistent,and 16 common peaks were identified.Except for Alxa Left Banner,Alxa Right Banner and Hetian City,the fingerprint similarities of samples between other producing areas and control fingerprint were greater than 0.9.The gallic acid,protocatechuic acid and catechin showed good linearity relationships within the ranges of 0.022–0.330,0.002–0.030,and 0.080–1.200μg;their correlation coefficients were 0.9998,0.9993 and 0.9994;their average recoveries were 100.54%,99.82%and 99.62%,with RSD of 1.71%,1.95%and 2.07%,respectively.The contents of gallic acid,protocatechuic acid and catechin of water fraction of Cynomorii Herba were 0.0313–7.0316,0.0255–0.3963,and 0.0035–0.7934 mg/g,respectively.The established PCA model could realize quality evaluation and classification of Cynomorii Herba in accordance with 12 city producing areas and 5 provi

关 键 词：锁阳 水溶性部位 高效液相色谱法 指纹图谱 同时测定 主成分分析 

分 类 号：R284.1[医药卫生—中药学]