摘要
建立山楂核药材的HPLC指纹图谱及含量测定方法。采用Welch Ultimate XB C;色谱柱(4.6 mm×250 mm, 5μm)进行分离,以乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱,流速1 mL·min^(-1),柱温30℃,进样量10μL,检测波长320 nm。采用上述色谱条件对不同产地的18批山楂核样品进行指纹图谱分析,共标定了24个共有峰,经对照品比对指认了其中3个主要色谱峰,并对这3个成分进行了同步含量测定。3个主要成分分别是erythro-(7S,8R)-guaiacylglycerol-β-coniferyl aldehyde ether、threo-(7R,8R)-guaiacylglycerol-β-coniferyl aldehyde ether和balanophonin。18批样品HPLC指纹图谱与对照指纹图谱的相对相似度介于0.928~0.999,3个成分的质量分数依次为0.055 1~0.182 7、0.061 8~0.225 8、0.156 8~0.405 6 mg·g^(-1)。采用SPSS 17.0和SIMCA 14.1软件对山楂核24个共有峰的峰面积进行聚类分析、主成分分析和正交偏最小二乘法判别分析,结果表明来自辽宁的2批样品与其他样品有较大差异,且3个待测成分均是导致山楂核差异的主要成分。该文所建立的方法操作简便、结果可靠,可用于山楂核的定性定量分析,研究结果为山楂核的质量控制提供了依据。
The purpose of this paper is to establish the HPLC fingerprint and content determination method for Crataegus pinnatifida seeds. The separation was developed on a Welch Ultimate XB C;column(4.6 mm×250 mm, 5 μm) by gradient elution with acetonitrile-water containing 0.1% formic acid as the mobile phase at the flow rate of 1 mL·min^(-1), the column temperature of 30 ℃, the injection volume of 10 μL, and the detection wavelength of 320 nm. Eighteen batches of samples were analyzed under the above chromatographic conditions to establish the fingerprint of C. pinnatifida seeds from different producing areas and a total of 24 common peaks were selected. The structures of three main chromatographic peaks were identified by comparison to reference substances, and the three compounds were simultaneously analyzed for content determination. They were identified as erythro-(7S,8R)-guaiacylglycerol-β-coniferyl aldehyde ether, threo-(7R,8R)-guaiacylglycerol-β-coniferyl aldehyde ether, and balanophonin, respectively. The relative similarity of fingerprints of 18 batches of samples and references ranged from 0.928 to 0.999, and the content of the three compounds was 0.055 1-0.182 7, 0.061 8-0.225 8, and 0.156 8-0.405 6 mg·g^(-1), respectively. SPSS 17.0 and SIMCA 14.1 were used for cluster analysis, principal component analysis(PCA), and orthogonal partial least squares discriminant analysis(OPLS-DA) on the common peaks of the HPLC fingerprint of C. pinnatifida seeds. The results showed that there were significant differences between the two batches of samples from Liaoning province and the other samples, and the three compounds to be tested were the main components leading to the difference of C. pinnatifida seeds. The established method was simple and reliable and can be used for qualitative and quantitative analysis of C. pinnatifida seeds. The findings of this study are expected to provide a scientific basis for quality control of C. pinnatifida seeds.
作者
杨悦
刘颖
冯伟红
刘晓谦
李春
王智民
YANG Yue;LIU Ying;FENG Wei-hong;LIU Xiao-qian;LI Chun;WANG Zhi-min(Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China)
出处
《中国中药杂志》
CAS
CSCD
北大核心
2022年第11期3000-3006,共7页
China Journal of Chinese Materia Medica
基金
国家重点研发计划“中医药现代化研究”重点专项(2017YFC1701900)。
关键词
山楂核
指纹图谱
含量测定
化学计量学
质量评价
Crataegus pinnatifida seeds
fingerprint
content determination
chemometrics
quality evaluation
