基于多模式识别结合UPLC指纹图谱及多指标成分定量测定的薏苡仁质量评价研究

Quality evaluation of Coicis Semen based on multiple pattern recognition combined with UPLC fingerprint and determination of mult-index component content determination

目的建立薏苡仁UPLC指纹图谱及多指标成分定量测定方法,并将薏苡仁UPLC指纹图谱、化学模式识别和多指标成分定量测定相结合,进而对不同产地薏苡仁药材进行综合质量评价。方法采用Waters C8色谱柱,以甲醇-纯水等度洗脱;体积流量0.2 mL/min;检测波长205 nm;柱温25℃;进样量0.3μL,建立15个不同产地薏苡仁药材指纹图谱,并进行相似度评价和化学模式识别;同时对不同产地薏苡仁药材进行一般性检查、浸出物测定及多个指标性成分含量测定。结果15个不同产地薏苡仁药材UPLC指纹图谱共标定14个共有峰,通过对照品指认了其中7个成分,包括三亚油酸甘油酯、1,2-二亚油酸-3-棕榈酸甘油酯、1,2-二亚油酸-3-油酸甘油酯、1-棕榈酸-2-油酸-3-亚油酸甘油酯、1,2-二油酸-3-亚油酸甘油酯、1,2-二油酸-3-棕榈酸甘油酯和三油酸甘油酯,上述7个成分重复性、稳定性及加样回收率结果均较好。此外,UPLC指纹图谱相似度范围为0.972~1.000;15个产地薏苡仁药材聚为3类,云南、福建样品聚为一类,贵州兴仁药材聚为一类,贵州兴义、安龙药材聚为一类;主成分综合得分表明云南、福建产地样品较优,通过筛选得出色谱峰2、5(三亚油酸甘油酯)、8和11(1,2-二油酸-3-棕榈酸甘油酯)是引起不同产地薏苡仁质量差异的主要成分;不同产地薏苡仁药材均符合《中国药典》2020年版水分、灰分和浸出物的标准;同时,多成分定量测定结果表明,7个指标性成分之间存在显著差异。结论建立了15个不同产地薏苡仁药材UPLC指纹图谱及含量测定方法,并结合UPLC指纹图谱、化学模式识别和多指标成分含量测定进行进一步研究,可为薏苡仁药材质量的综合评价提供参考。

Objective To establish a method for the UPLC fingerprint and multi-indicator component content determination of Yiyiren(Coicis Semen),and to combine the UPLC fingerprint of Coicis Semen,chemical pattern recognition,and multi-indicator component content determination with the aim of evaluating the quality of Coicis Semen herbs from different origins.Methods A Waters C8 column was used with isocratic elution of methanol-pure water;the flow rate was 0.2 mL/min;the detection wavelength was 205 nm;the column temperature was 25℃;the injection volume was 0.3μL;the fingerprints of 15 Coicis Semen herbs of different origins were established;the similarity evaluation and chemical pattern recognition were carried out;At the same time,the herbs of different origins of Coicis Semen were subjected to general examination,determination of leachate and determination of the content of several index components.Results A total of 14 common peaks were identified in the UPLC fingerprints of 15 herbs of different origins of Coicis Semen,and seven of them were identified by the control,including trilinolein(LLL),1,2-dilinoleoyl-3-palmitoyl-glycerol(OOP),1,2-dilinoleoyl-3-oleoyl-glycerol,1-palmitoyl-2-oleoyl-3-linoleoyl-glycerol,1,2-dioleoyl-3-linoleoyl-glycerol,1,2-dioleoyl-3-palmitoyl-glycerol,and triolein,the results of reproducibility,stability and spiked recoveries of the above seven components were good.In addition,the similarity of UPLC fingerprints ranged from 0.972 to 1.000;the 15 origin Coicis Semen herbs were clustered into three categories,the samples from Yunnan and Fujian were clustered into one category,the herbs from Xingren of Guizhou were clustered into one category,and the herbs from Xingyi and Anlong of Guizhou were clustered into one category;the composite scores of the principal components indicated that the samples of Yunnan and Fujian origins were superior,and the chromatographic peaks 2,5(LLL),8 and 11(OOP)obtained by screening were the main components that caused the quality differences of Coicis Semen from different origins;the herbs of Coicis Semen from different origins complied with the standards of moisture,ash and leachate in the 2020 edition of the Chinese Pharmacopoeia;meanwhile,the results of multi-component quantitative determination showed that there were significant differences between the seven index components.Conclusion The study established the UPLC fingerprints of 15 Coicis Semen herbs from different origins and their content determination methods,and combined with UPLC fingerprints,chemical pattern recognition,and multi-indicator component content determination for further research,which can provide a reference for the comprehensive evaluation of the quality of Coicis Semen herbs.