近红外光谱技术快速测定三七水分和醇溶性浸出物
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摘要
目的利用近红外光谱技术(near infrared spectroscopy,NIRS)建立三七药材水分和醇溶性浸出物定量分析的快速测定方法。方法参照《中国药典》2015年版三七水分和醇溶性浸出物含量测定方法对53批药材分别测定水分和醇溶性浸出物含量,采用偏最小二乘法(PLS)分别建立水分和醇溶性浸出物的近红外定量分析模型,并利用内部交叉验证和外部验证的方法对模型进行优化。结果药材样品中水分和醇溶性浸出物预测最佳波段分别为4 450.32~7 350.01 cm-1和6 163.92~3 984.71 cm-1。定量模型校正集相关系数分别为0.997 2和0.962 4,校正均方差分别为0.039 6和0.776 0;验证集的相关系数为0.962 4和0.988 4,验证均方差分别为0.173和0.595。结论该方法准确、快速、无污染,可用于三七药材中水分和醇溶性浸出物含量的快速测定。
Objective This study aimed at establishing the quantitative model of moisture and ethanol extract content in Panax notoginseng by NIRS. Methods Oven drying method of Chinese Pharmacopoeia 2015 was used to determine the moisture and ethanol extract content of 53 samples. The correlation models of the NIR spectra and the reference values of moisture and ethanol extract content were obtained with partial least square(PLS) method and optimized through inner cross validation and external validation. Results The optimal spectrum range of moisture and ethanol extract were 4 450.32—7 350.01 cm-1 and 6 163.92—3984.71 cm-1. The correlation coefficients of calibration for moisture and ethanol extract were 0.997 2 and 0.962 4,and the root mean square errors of calibration were 0.039 6 and 0.776 0. The correlation coefficients of predication were 0.962 4 and 0.988 4, and the root mean square errors of prediction were 0.173 and 0.595. Conclusion The presented method is accuracy, timesaving and nondestructive, which could be applied for the rapid detection of the moisture and ethanol extract content in Panax notoginseng.
Objective This study aimed at establishing the quantitative model of moisture and ethanol extract content in Panax notoginseng by NIRS. Methods Oven drying method of Chinese Pharmacopoeia 2015 was used to determine the moisture and ethanol extract content of 53 samples. The correlation models of the NIR spectra and the reference values of moisture and ethanol extract content were obtained with partial least square(PLS) method and optimized through inner cross validation and external validation. Results The optimal spectrum range of moisture and ethanol extract were 4 450.32—7 350.01 cm-1 and 6 163.92—3984.71 cm-1. The correlation coefficients of calibration for moisture and ethanol extract were 0.997 2 and 0.962 4,and the root mean square errors of calibration were 0.039 6 and 0.776 0. The correlation coefficients of predication were 0.962 4 and 0.988 4, and the root mean square errors of prediction were 0.173 and 0.595. Conclusion The presented method is accuracy, timesaving and nondestructive, which could be applied for the rapid detection of the moisture and ethanol extract content in Panax notoginseng.
引文
[1]中国药典[S].一部. 2015.
[2]李真,周立红,叶正良,等.近红外光谱分析技术在药物质量分析中的应用进展[J].药物评价研究, 2016(4):686-692.
[3]马越,刘永强,门宇凤,等.近红外光谱法快速测定芍药根中芍药苷和芍药内酯苷[J].中草药, 2018, 49(3):700-707.
[4]Navarro E M, Rodenas S F, Li H, et al. Rapid determination of baicalin and total baicalein content in Scutellariae Radix by ATR-IR and NIR spectroscopy[J].Talanta, 2013, 114(10):304-310.
[5]闫珂巍,陈美君,梅国荣,等.近红外光谱法测定三七中3种皂苷的总含量[J].药物分析杂志, 2016, 36(4):691-696.
[6]杨南林,瞿海斌,程翼宇.近红外光谱法快速测定三七总皂苷的方法研究[J].浙江大学学报, 2002, 36(4):464-466.
[7]杨南林,程翼宇,吴永江.中药材三七中皂苷类成分的近红外光谱快速无损分析新方法[J].化学学报, 2013,61(3):393-398.
[8]陆婉珍.现代近红外光谱分析技术[M].第二版.北京:中国石化出版社, 2007.
[9]Zhang X B, Feng Y C, Hu C Q.Feasibility and extension of universal quantitative models for moisture content determination in beta-lac-tam powder injections by nearinfrared spectroscopy[J]. Analytica Chimica Acta, 2008,630(2):131-140.
[10]李化,柯华香,贺敬霞,等.近红外漫反射光谱结合偏最小二乘法快速测定厚朴中酚类成分和水分含量[J].中国实验方剂学杂志, 2015, 21(22):72-76.
[2]李真,周立红,叶正良,等.近红外光谱分析技术在药物质量分析中的应用进展[J].药物评价研究, 2016(4):686-692.
[3]马越,刘永强,门宇凤,等.近红外光谱法快速测定芍药根中芍药苷和芍药内酯苷[J].中草药, 2018, 49(3):700-707.
[4]Navarro E M, Rodenas S F, Li H, et al. Rapid determination of baicalin and total baicalein content in Scutellariae Radix by ATR-IR and NIR spectroscopy[J].Talanta, 2013, 114(10):304-310.
[5]闫珂巍,陈美君,梅国荣,等.近红外光谱法测定三七中3种皂苷的总含量[J].药物分析杂志, 2016, 36(4):691-696.
[6]杨南林,瞿海斌,程翼宇.近红外光谱法快速测定三七总皂苷的方法研究[J].浙江大学学报, 2002, 36(4):464-466.
[7]杨南林,程翼宇,吴永江.中药材三七中皂苷类成分的近红外光谱快速无损分析新方法[J].化学学报, 2013,61(3):393-398.
[8]陆婉珍.现代近红外光谱分析技术[M].第二版.北京:中国石化出版社, 2007.
[9]Zhang X B, Feng Y C, Hu C Q.Feasibility and extension of universal quantitative models for moisture content determination in beta-lac-tam powder injections by nearinfrared spectroscopy[J]. Analytica Chimica Acta, 2008,630(2):131-140.
[10]李化,柯华香,贺敬霞,等.近红外漫反射光谱结合偏最小二乘法快速测定厚朴中酚类成分和水分含量[J].中国实验方剂学杂志, 2015, 21(22):72-76.