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不同产地皂角刺多指标定量检测及质量差异评价
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| 篇名： | 不同产地皂角刺多指标定量检测及质量差异评价 |
| TITLE： | Multi-index quantitative detection and quality difference evaluation of Gleditsia sinensis from different producing areas |
| 摘要： | 目的 建立不同产地皂角刺的多指标定量检测方法，并评价其质量差异。方法采用高效液相色谱-一测多评（HPLC-QAMS）法同时检测皂角刺中原儿茶酸、香草酸、异东莨菪内酯、滨蒿内酯、异牡荆素、黄颜木素、花旗松素、漆黄素、槲皮素、山柰酚、刺囊酸、白桦脂酸、β-谷甾醇、豆甾醇的含量，色谱柱为KromasilC18，流动相为0.2%磷酸-乙腈溶液（梯度洗脱），检测波长针对不同指标成分分别为254、360、210nm，柱温为30℃，流速为1.0mL/min，进样量为10μL；按照《中国药典》方法检测浸出物和总灰分含量；利用化学计量学、加权逼近理想解排序（TOPSIS）分析、Logistic回归模型对不同产地30批（编号S1～S30）皂角刺样品进行质量差异评价。结果上述14种成分依次在1.55～77.50、0.71～35.50、0.28～14.00、0.96～48.00、1.77～88.50、0.09～4.50、4.65～232.50、1.49～74.50、0.37～18.50、1.18～59.00、7.35～367.50、3.58～179.00、0.49～24.50、0.21～10.50μg/mL质量浓度范围内线性关系良好（r均大于0.999），精密度、稳定性（24h）及重复性的RSD均小于2.00%，平均加样回收率为96.99%～100.13%（RSD均小于2.00%），相对校正因子重复性良好。浸出物和总灰分含量分别为4.2%～12.5%和0.5%～2.3%。QAMS法与外标法所测得的14种成分的含量差异无统计学意义（P＞0.05）。化学计量学分析结果显示，30批皂角刺样品可聚为3类，其中S1～S11聚为一类，S12～S20聚为一类，S21～S30聚为一类；刺囊酸、白桦脂酸、花旗松素、山柰酚、异牡荆素、滨蒿内酯和原儿茶酸可能是影响不同产地皂角刺质量的差异成分。加权TOPSIS分析结果显示，30批皂角刺的相对贴近度（Jb）为0.1445～0.7218，其中样品S27的质量最优（Jb值为0.7218）。Logistic回归模型分析结果显示，样品S21～S30为优级，S1～S11为中级，S12～S20为差级。结论所建立的HPLC-QAMS法操作简便、结果准确，综合评价方法客观、全面，可用于不同产地皂角刺的质量差异评价。 |
| ABSTRACT： | OBJECTIVE To establish a multi-index quantitative detection method， and to evaluate the quality difference of Gleditsia sinensis from different producing areas. METHODS The contents of protocatechuic acid， vanillic acid， isoscopoletin， scoparone， isovitexin， fustin， taxifolin， fisetin， quercetin， kaempferol， echinocystic acid， betulinic acid， β -sitosterol and stigmasterol were detected by high performance liquid chromatography-quantitative analysis of multi-components by single marker （HPLC-QAMS）. The chromatographic column was Kromasil C18， the mobile phase was 0.2% phosphoric acid-acetonitrile solution （gradient elution）， the detection wavelengths were 254， 360， 210 nm for different index components， the column temperature was 30 ℃ ， the flow rate was 1.0 mL/min， and the sample injection volume was 10 μL. The contents of extract and total ash were detected according to the method of Chinese Pharmacopoeia. The quality differences of 30 batches of G. sinensis （No. S1-S30） from different producing areas were evaluated by chemometrics， weighted technique for order preference by similarity to an ideal solution （TOPSIS） analysis and Logistic regression model. RESULTS The linear ranges of 14 components were 1.55-77.50， 0.71- 35.50， 0.28-14.00， 0.96-48.00， 1.77-88.50， 0.09-4.50， 4.65-232.50， 1.49-74.50， 0.37-18.50， 1.18-59.00， 7.35-367.50， 3.58- 179.00， 0.49-24.50 and 0.21-10.50 μg/mL， respectively （all r＞0.999）. The RSDs of precision， stability （24 h） and repeatability were less than 2.00%； the average recoveries were 96.99%-100.13% （all RSDs＜2.00%）， and the relative correction factor had good repeatability. The contents of extract and total ash were Δ 基金项目 湖北省中医药科研立项青年人才项目 （No. 4.2%-12.5% and 0.5%-2.3%， respectively. There was no ZY2019Q014） significant difference in the content of 14 components measured by QAMS method and external standard method （P＞0.05）. The results of chemometrics showed that 30 batches of samples were clustered into 3 categories： S1 to S11 form one category， S12 to S20 form another category， and S21 to S30 constitute the third category. Echinocystic acid， betulinic acid， taxifolin， kaempferol， isovitexin， scoparone and protocatechuic acid may be the differential components affecting the quality of G. sinensis from different producing areas. The analysis results of the weighted TOPSIS method revealed that relative closeness （Jb） for 30 batches of G. sinensis ranged from 0.144 5 to 0.721 8， with S27 achieving the highest value （Jb） of 0.721 8. The analysis results of the Logistic regression model showed that S21-S30 batches of samples were of superior grade， S1-S11 were of intermediate grade， and S12-S20 were of inferior grade. CONCLUSIONS The established HPLC-QAMS method is simple and accurate. The comprehensive evaluation method is objective and comprehensive， and can be used to evaluate the quality difference of G. sinensis from different producing areas. |
| 期刊： | 2025年第36卷第05期 |
| 作者： | 梁美锋；万雄飞；廖念；朱珊珊；王志坚 |
| AUTHORS： | LIANG Meifeng，WAN Xiongfei，LIAO Nian，ZHU Shanshan，WANG Zhijian |
| 关键字： | 皂角刺；高效液相色谱法；一测多评法；化学计量学；加权TOPSIS分析；Logistic回归模型；质量差异评价 |
| KEYWORDS： | Gleditsia sinensis； HPLC； QAMS； chemometrics； weighted TOPSIS； Logistic regression model； quality difference |
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