摘要
目的建立柚核高效液相色谱(high performance liquid chromatography,HPLC)指纹图谱和多指标成分质量分数测定方法,并结合化学模式进行识别,评价不同产地柚核质量。方法采用Shim-pack GIST C_(18)(4.6 mm×150 mm,5μm)色谱柱;以乙腈-0.3%磷酸为流动相梯度洗脱,检测波长为210 nm;流速为1.0 mL/min;柱温为30℃;进样量为20μL,建立柚核HPLC指纹图谱。采用主成分分析(principal component analysis,PCA)、聚类分析(cluster analysis,CA)、正交偏最小二乘法判别分析(orthogonal partial least squares-discriminant analysis,OPLS-DA)对不同产地柚核进行质量评价。结果10批柚核样品指纹图谱与对照指纹图谱(R)的相似度均高于0.95,各批次间相似度均在0.90以上,共标定了11个共有峰,指认了其中5种成分。通过化学模式识别分析将10批样品聚类为2类,与产地信息一致,并确立了6个差异性标志物,对其中已指认的4种成分进行质量分数测定。柚皮苷、柠檬苦素、诺米林、黄柏酮质量分数分别为0.019%~0.120%、0.519%~0.757%、0.379%~0.539%、0.031%~0.055%。结论本研究建立的指纹图谱及质量分数测定方法专属性强、稳定性高,可用于柚核药材的质量评价。
Objective To establish an HPLC fingerprint and multi index component content determination method for Citrus grandis Seeds,and evaluate the quality of Citrus grandis Seeds from different origins by combining chemical pattern recognition.Methods A fingerprint method was established by a Shim-pack GIST C_(18)column(4.6 mm×150 mm,5μm)with a mobile phase of acetonitrile-0.3%phosphoric acid aqueous solution under gradient elution.The detection wavelength was 210 nm,flow rate was 1.0 mL/min,column temperature was 30℃,and injection volume was 20μL.Principal component analysis(PCA),cluster analysis(CA),and orthogonal partial least squares-discriminant analysis(OPLS-DA)were employed for quality assessment.Results The similarities between the fingerprints of 10 batches of Citrus grandis seed samples and the reference fingerprint(R)were all higher than 0.95,while inter-batch similarities exceeded 0.938.Eleven common peaks were calibrated,with five components identified.Chemical pattern recognition analysis clustered the samples into two categories,which were consistent with their origin information.Six differential markers were identified,and quantitative analysis was performed on four of the identified components.The multi-component quantitative results demonstrated the following content ranges:naringin 0.019%-0.120%,limonin 0.519%-0.757%,nomilin 0.379%-0.539%,and obacunone 0.031%-0.055%.Conclusion The established fingerprint and quantitative methods exhibit strong specificity and high stability,which can be used for the quality evaluation of Citrus grandis seed medicinal material.
作者
古炳明
杨勋
姚海燕
李艳媚
马泽扬
陈永颐
刘佳
GU Bingming;YANG Xun;YAO Haiyan;LI Yanmei;MA Zeyang;CHEN Yongyi;LIU Jia(Meizhou Institute for Food and Drug Control,Meizhou 514011,China;School of Medicine,Jiaying University,Meizhou 514011,China)
出处
《广东药科大学学报》
2025年第6期92-98,共7页
Journal of Guangdong Pharmaceutical University
基金
广东省药品检验所科研项目(SN2024037)
广东省药品监督管理局科技创新项目(2023TDB29)。
关键词
柚核
指纹图谱
化学模式识别
含量测定
Citrus grandis Seeds
fingerprint
chemical pattern recognition
content determination
