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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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近红外光谱法快速测定锁阳中多指标成分含量

Rapid determination of multi-index components in Cynomorii Herba by NIR

分类号:R917
出版年·卷·期(页码):2020,40 (6):1076-1089
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的: 建立锁阳中没食子酸、原儿茶酸、儿茶素、总多糖、总黄酮含量的近红外光谱(NIR)定量分析模型,实现锁阳中多指标成分含量的快速测定。方法: 收集5个省不同产地的101批锁阳样品,没食子酸、原儿茶酸、儿茶素含量的化学参考值采用HPLC法同时测定,总多糖、总黄酮含量的化学参考值采用紫外分光光度法测定,以积分球漫反射方式采集NIR原始光谱,采用化学计量学方法对原始光谱进行预处理,选择最佳波段及主因子数,以偏最小二乘(PLS)法建立NIR定量分析模型。结果: 所建没食子酸定量校正模型的R2为0.963 4,RMSEC为0.651 8,RMSEP为0.607 6;交叉验证R2为0.914 9,RMSECV为0.898 7;外部验证相对误差在0.84%~7.0%内,平均回收率为101.6%。原儿茶酸R2为0.957 1,RMSEC为0.798 3,RMSEP为0.465 2;交叉验证R2为0.927 5,RMSECV为0.976 0;外部验证相对误差在1.8%~6.3%内,平均回收率为99.6%。儿茶素R2为0.947 6,RMSEC为0.408 6,RMSEP为0.413 9;交叉验证R2为0.920 7,RMSECV为0.578 3;外部验证相对误差在1.1%~6.6%内,平均回收率为98.9%。总黄酮R2为0.925 7,RMSEC为0.835 9,RMSEP为0.796 4;交叉验证R2为0.908 1,RMSECV为0.885 1;外部验证相对误差在0.19%~6.3%内,平均回收率为101.8%。总多糖R2为0.932 9,RMSEC为0.265 3,RMSEP为0.251 1;交叉验证R2为0.893 9,RMSECV为0.387 3;外部验证相对误差在0.44%~6.1%内,平均回收率为102.1%。结论: 所建模型预测结果准确、可靠,本法操作简单、快速,可用于锁阳中没食子酸、原儿茶酸、儿茶素、总多糖、总黄酮的定量分析。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To establish the near-infrared spectroscopy(NIR)quantitative analysis models for the contents of gallic acid,protocatechuic acid,catechin,total flavonoids,and total polysaccharides in Cynomorii herba,so as to achieve rapid determination of multi-index components in Cynomorii Herba.Methods: 101 batches of Cynomorii Herba from different habitats in 5 provinces were collected.The chemical reference values of gallic acid,protocatechuic acid,and catechin were simultaneously determined by HPLC and total flavonoids and total polysaccharides were determined by UV spectrophotometry.The original NIR spectra were collected by integral sphere diffuse reflection and preprocessed by chemometrics methods.The optimal spectral ranges and factors were selected,and the NIR quantitative analysis models were established by partial least squares(PLS)method.Results: The parameters of the established quantitative model for gallic acid were as follows:R2=0.963 4,RMSEC=0.651 8,RMSEP=0.607 6;R2=0.914 9,RMSECV=0.898 7 for cross validation;the relative error was within 0.84%-7.0%,and average recovery was 101.6% for external verification.The parameters of model for protocatechuic acid were as follows:R2=0.957 1,RMSEC=0.798 3,RMSEP=0.465 2;R2=0.927 5,RMSECV=0.976 0 for cross validation;the relative error was within 1.7%-6.3%,and average recovery was 99.6% for external verification.The parameters of model of catechin were as follows:R2=0.947 6,RMSEC=0.408 6,RMSEP=0.413 9;R2=0.920 7,RMSECV=0.578 3 for cross validation;the relative error was within 1.1%-6.6%,and average recovery was 98.9% for external verification.The parameters of model of total flavonoids were as follows:R2=0.925 7,RMSEC=0.835 9,RMSEP=0.796 4;R2=0.908 1,RMSECV=0.885 1 for cross validation;the relative error was within 0.19%-6.33%,and average recovery was 101.8% for external verification.The parameters of model of total polysaccharides were as follows:R2=0.932 9,RMSEC=0.265 3,RMSEP=0.251 1;R2=0.893 9,RMSECV=0.387 3 for cross validation;the relative error was within 0.44%-6.1%,and average recovery was 102.1% for external verification.Conclusion: The established models in this study were accurate,reliable,simple and rapid.It can be used to quantitatively analyze the contents of gallic acid,protocatechuic acid,catechin,total flavonoids,and total polysaccharids in Cynomorii Herba.

-----参考文献:---------------------------------------------------------------------------------------
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