[关键词]
[摘要]
目的 建立牛尾菜Smilax riparia中香草酸、异香草酸、鼠李素、木犀草素、槲皮素、香叶木素、齐墩果酸、熊果酸、知母皂苷A2、纤细薯蓣皂苷、薯蓣次皂苷A、薯蓣皂苷、原纤细薯蓣皂苷、β-谷甾醇、豆甾醇、总灰分和酸不溶性灰分含量测定方法,结合多元统计分析及熵权TOPSIS模型对牛尾菜质量进行综合评价。方法 采用Symmetry C18色谱柱(250 mm×4.6mm,5μm),乙腈-0.3%磷酸水溶液为流动相,梯度洗脱,体积流量1.0 mL/min;柱温30℃;检测波长280 nm(检测香草酸和异香草酸)、345 nm(检测鼠李素、木犀草素、槲皮素和香叶木素)、210 nm(检测齐墩果酸、熊果酸、知母皂苷A2、纤细薯蓣皂苷、薯蓣次皂苷A、薯蓣皂苷、原纤细薯蓣皂苷、β-谷甾醇和豆甾醇);进样量10μL。按照《中国药典》2025年版方法检测总灰分和酸不溶性灰分含量。基于含量测量值,采用多元统计分析和熵权-TOPSIS模型对18批样品质量进行综合评价。结果 15个化学成分分别在各自质量浓度范围内线性关系良好,平均加样回收率为96.99%~100.14%,18批牛尾菜中香草酸、异香草酸、鼠李素、木犀草素、槲皮素、香叶木素、齐墩果酸、熊果酸、知母皂苷A2、纤细薯蓣皂苷、薯蓣次皂苷A、薯蓣皂苷、原纤细薯蓣皂苷、β-谷甾醇、豆甾醇、总灰分和酸不溶性灰分质量分数分别为0.338~1.213、0.074~0.200、0.197~0.360、0.423~0.676、0.620~1.814、0.496~1.007、0.192~0.410、0.095~0.187、1.360~2.281、0.379~0.651、0.711~1.221、2.120~3.657、0.965~1.652、0.113~0.275、0.063~0.123 mg/g及3.6%~9.5%、1.4%~3.5%;通过多元统计分析将18批牛尾菜分为3类,主成分分析得到2个主成分,累积方差贡献率为88.149%,通过变量权重值筛选出薯蓣皂苷、槲皮素、木犀草素、知母皂苷A2、齐墩果酸、香草酸、原纤细薯蓣皂苷和β-谷甾醇可作为不同产地牛尾菜为的差异标志物;熵权TOPSIS法结果显示18批牛尾菜质量差异显著,综合得分为0.230 6~0.706 2,其中编号为S16和S15的样品质量排序靠前。结论 基于化学计量学和熵权-TOPSIS的建立的质量评价模型方便有效,可用于牛尾菜质量评价。
[Key word]
[Abstract]
Objective To develop the determination methods for the content of vanillic acid, isovanillic acid, rhamnetin, luteolin, quercetin, diosmetin, oleanolic acid, ursolic acid, anemarrhenasaponin A2, gracillin, prosapogenin A, dioscin, protogracillin, β-sitosterol, stigmasterol, total ash and acid insoluble ash in Smilax riparia, and evaluate the quality of S. riparia by combining multivariate statistical analysis and entropy weight TOPSIS model. Methods HPLC was launched on an Agilent Symmetry C18 chromatographic column(250 mm×4.6 mm,5 μm) by gradient elution with a mobile phase of acetonitrile-0.3% phosphoric acid at a flow rate of 1.0 mL/min, detection wavelength were 280 nm(for detecting vanillic acid and isovanillic acid), 345 nm(for detecting rhamnetin, luteolin, quercetin, diosmetin) and 210 nm(for detecting oleanolic acid, ursolic acid, anemarrhenasaponin A2, gracillin, prosapogenin A, dioscin, protogracillin, β-sitosterol, stigmasterol), column temperature was 30 ℃, and an injection volume was 10 μL. The contents of total ash and acid insoluble ash were detected according to the method of Chinese Pharmacopoeia 2025 edition. Based on the content measurement value, the quality of 18 batches of S. riparia samples was comprehensively evaluated by using the multivariate statistical analysis and entropy weight TOPS model. Results A total of 15 chemical components had good linear relationships in their respective mass concentration ranges, and the average recovery rates were 96.99%—100.14%. The contents of vanillic acid, isovanillic acid, rhamnetin, luteolin, quercetin, diosmetin, oleanolic acid, ursolic acid, anemarrhenasaponin A2, gracillin, prosapogenin A, dioscin, protogracillin, β-sitosterol, stigmasterol, total ash and acid insoluble ashin in 18 batches of S. riparia were 0.338—1.213, 0.074—0.200, 0.197—0.360, 0.423—0.676, 0.620—1.814, 0.496—1.007, 0.192—0.410, 0.095—0.187, 1.360—2.281, 0.379—0.651, 0.711—1.221, 2.120 —3.657, 0.965—1.652, 0.113—0.275, 0.063—0.123 mg/g, 3.6%—9.5%, 1.4%—3.5%, respectively. Multivariate statistical analysis classified 18 batches of S. riparia into three categories, principal component analysis yielded two principal components, with a cumulative variance contribution rate of 88.149%. A total of eight components such as dioscin, quercetin, luteolin, anemarrhenasaponin A2, oleanolic acid, vanillic acid, protogracillin and β-sitosterol were screened by VIP analysis, which could be used as differential markers of S. riparia in different producing areas. The results of entropy weight TOPSIS method showed that the quality of 18 batches of S. riparia was significantly different, and the comprehensive score was 0.230 6—0.706 2. The quality of samples numbered S16 and S15 was ranked in the front. Conclusion The quality evaluation model based on chemometrics and entropy weight TOPSIS is convenient and effective, and can be used for the quality evaluation of S. riparia.
[中图分类号]
R286.2
[基金项目]
国家自然科学基金面上项目(82074026);江西省教育厅科学技术研究项目(GJJ211236)