近红外光谱法快速检测赤芍配方颗粒芍药苷和浸出物含量
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摘要
为了直接、快速地测定赤芍配方颗粒中芍药苷和浸出物的含量,解决回流烘干法测定耗时长、操作繁琐等问题,利用近红外漫反射技术,结合偏最小二乘法(PLS),建立了测定芍药苷和浸出物含量的近红外光谱测定方法。选用积分球系统测定样品的近红外光谱,定量模型的预处理方法采用多元散射校正和一阶导数进行处理,光谱范围分别为5 492～5 103cm-1,7 428～7 201cm-1,6 942～5 322cm-1。结果表明,定量模型中芍药苷含量和浸出物含量的最佳主因子数分别为7和6,内部交叉验证均方差分别为0.082 6和0.226 0,决定系数(R2)分别为0.981 7和0.982 4,系统精密度RSD值分别为1.1%和0.9%,方法精密度RSD值分别为2.1%和1.6%,外部验证预测均方差分别为0.363和0.282。采用建立的近红外预测模型对赤芍配方颗粒进行快速测定,方法可行,分析快速、简便,结果准确,为赤芍配方颗粒的测定提供了高效方法。
In order to directly and quickly determine paeoniflorin and its extraction content in Paeoniae Radix Rubra formula granules and solve the problems of long time consuming and complicated operation of reflux drying method,a near infrared spectroscopy method for determining paeoniflorin content and extraction content is established by using near infrared diffuse reflectance technology and partial least squares(PLS).The near infrared spectrum of the sample is determined by an integrating sphere system,and the pretreatment method of the quantitative model is processed by multiple scattering correction and first derivative.The wavelength range is 5 492～5 103cm-1,7 428～7 201cm-1,6 942～5 322cm-1,respectively.The results show that the numbers of the best principal factors for the amount of paeoniflorin and the amount of leachate in the quantitativemodel are 7and 6,and the internal mean cross-validation variances are 0.082 6and 0.226 0,the coefficients of determination(R2)are 0.981 7and 0.982 4,while the system precision RSDs are 1.1%and 0.9%,and the method precision RSD are 2.1%and 1.6%.The external verification predicted mean variances are 0.363 and 0.282.The established near infrared prediction model is used to quickly determine the Paeoniae Radix Rubra formula granules.The method is feasible,rapid,simple and accurate,and provides an efficient method for the determination of the Paeoniae Radix Rubra formula granules.
In order to directly and quickly determine paeoniflorin and its extraction content in Paeoniae Radix Rubra formula granules and solve the problems of long time consuming and complicated operation of reflux drying method,a near infrared spectroscopy method for determining paeoniflorin content and extraction content is established by using near infrared diffuse reflectance technology and partial least squares(PLS).The near infrared spectrum of the sample is determined by an integrating sphere system,and the pretreatment method of the quantitative model is processed by multiple scattering correction and first derivative.The wavelength range is 5 492～5 103cm-1,7 428～7 201cm-1,6 942～5 322cm-1,respectively.The results show that the numbers of the best principal factors for the amount of paeoniflorin and the amount of leachate in the quantitativemodel are 7and 6,and the internal mean cross-validation variances are 0.082 6and 0.226 0,the coefficients of determination(R2)are 0.981 7and 0.982 4,while the system precision RSDs are 1.1%and 0.9%,and the method precision RSD are 2.1%and 1.6%.The external verification predicted mean variances are 0.363 and 0.282.The established near infrared prediction model is used to quickly determine the Paeoniae Radix Rubra formula granules.The method is feasible,rapid,simple and accurate,and provides an efficient method for the determination of the Paeoniae Radix Rubra formula granules.
引文
[1]国家药典委员会.中华人民共和国药典(一部)[M].北京:中国医药科技出版社,2015.
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[11]李军山,高晗,张肖建,等.近红外光谱法快速测定猪去氧胆酸含量[J].中国现代中药,2016,18(5):588-590.LI Junshan,GAO Han,ZHANG Xiaojian,et al.Rapid quantitative analysis of hyodeoxycholic acid by near infrared spectroscopy[J].Modern Chinese Medicine,2016,18(5):588-590.
[12]郝磊,李军山,彭新华,等.丹参药材水分近红外定量模型的建立[J].中国药物警戒,2016,13(8):464-467.HAO Lei,LI Junshan,PENG Xinhua,et al.Establishment of rapid analysis of water in Salvia Miltiorrhiza by near infrared diffuse reflectance spectroscopy[J].Chinese Journal of Pharmacovigilance,2016,13(8):464-467.
[13]刘国海,韩蔚强,江辉.基于近红外光谱的橄榄油品质鉴别方法研究[J].光谱学与光谱分析,2016,36(9):2798-2801.LIU Guohai,HAN Weiqiang,JIANG Hui.Study on quality identification of olive oil based on near infrared spectra[J].Spectroscopy and Spectral Analysis,2016,36(9):2798-2801.
[14]YUN Yonghuan,WANG Weiting,TAN Minli,et al.A strategy that iteratively retains informative variables for selecting optimal variable subset in multivariate calibration[J].Analytica Chimica Acta,2014,807(1):36-43.
[15]谢越,周成,涂从,等.近红外光谱技术定量分析连作滁菊土壤中的阿魏酸含量[J].分析化学,2017,45(3):363-368.XIE Yue,ZHOU Cheng,TU Cong,et al.Quantitative determination of ferulic acid content in Chrysanthemum Morifolium cv(Chuju)continuous cropping soil using near infrared spectroscopy[J].Chinese Journal of Analytical Chemistry,2017,45(3):363-368.
[16]乔瑶瑶,赵武奇,胡新中,等.近红外光谱技术检测燕麦中蛋白质含量[J].中国粮油学报,2016,31(8):138-142.QIAO Yaoyao, ZHAOWuqi, HUXinzhong,etal.Determination of protein content in oat using near-infrared spectroscopy[J].Journal of the Chinese Cereals and Oils Association,2016,31(8):138-142.
[17]商志伟,赵云,沈奇,等.紫苏种子品质的近红外光谱分析[J].光谱学与光谱分析,2017,37(12):3719-3724.SHANG Zhiwei,ZHAO Yun,SHEN Qi,et al.Quality analysis with near-infrared spectroscopy in Perilla seed[J].Spectroscopy and Spectral Analysis,2017,37(12):3719-3724.
[18]张金伟,张延莹,刘岩,等.近红外光谱法在线质量监控白芍工业化提取[J].中草药,2011,42(12):2459-2461.ZHANG Jinwei,ZHANG Yanying,LIU Yan,et al.On-line quality control for Paeoniae Radix Alba industrial extraction by NIRS[J].Chinese Traditional and Herbal Drugs,2011,42(12):2459-2461.
[19]李军山,陈钟,彭新华,等.杜仲不同炮制品配方颗粒红外快速鉴别[J]河北工业科技,2016,33(6):503-508.LI Junshan,CHEN Zhong,PENG Xinhua,et al.Rapid identification of different processed products of Eucommia ulmoides formula granules by FTIR[J].Hebei Journal of Industrial Science and Technology,2016,33(6):503-508.
[2]陆婉珍.现代近红外光谱分析技术[M].北京:中国石化出版社,2007.
[3]白铁成,王亚明,张楠楠,等.胡杨叶片水分含量的近红外光谱检测[J].光谱学与光谱分析,2017,37(11):3419-3423.BAI Tiecheng,WANG Yaming,ZHANG Nannan,et al.Near infrared spectrum detection method for moisture content of Popuius Euphratica leaf[J].Spectroscopy and Spectral Analysis,2017,37(11):3419-3423.
[4]高晗,李军山,郝鹏彬,等.近红外光谱法快速测定侧柏叶配方颗粒槲皮苷含量[J].中国现代中药,2015,17(7):722-725.GAO Han,LI Junshan,HAO Pengbin,et al.Rapid quantitative aanlysis of quercetin-3-rhamnoside in Cacumen Platicladi formula granules by near infrared diffuse reflectance spectroscopy[J].Modern Chinese Medicine,2015,17(7):722-725.
[5]李军山,张博,校军彦.近红外光谱法快速测定大豆磷脂粉的干燥失重及磷含量[J].中国药业,2013,22(16):41-43.
[6]李军山,陈钟,张博.近红外光谱技术监控银杏叶提取物柱层析的研究[J].药物分析杂志,2014,34(11):2098-2101.LI Junshan,CHEN Zhong,ZHANG Bo.Study on monitoring column chromatography of Ginkgo biloba extract by near infrared spectroscopy[J].Chinese Journal of Pharmaceutical Analysis,2014,34(11):2098-2101.
[7] LI Junshan,ZHANG Bo.Extraction process validation of Isatis Radix[J].Pharmacology&Pharmacy,2014,5:356-363.
[8]高会芹,李军山,李振江,等.红参提取工艺近红外光谱与液相色谱比较研究[J].药物分析杂志,2015,35(7):1274-1278.GAO Huiqin,LI Junshan,LI Zhenjiang,et al.Comparative study of near infrared spectroscopy and liquid chromatography for Red Ginseng extraction process[J].Chinese Journal of Pharmaceutical Analysis,2015,35(7):1274-1278.
[9]李军山,彭新华,张博.近红外光谱法快速测定茯苓药材水分[J].亚太传统医药,2011,7(8):36-38.LI Junshan,PENG Xinhua,ZHANG Bo.Studies on rapid quantitative analysis of the water in Poria Cocos by infrared diffuse reflectance spectroscopy[J].Asia-Pacific Traditional Medicine,2011,7(8):36-38.
[10]陈钟,李军山,彭新华.近红外光谱法快速测定利咽解毒颗粒中黄芩苷含量[J].亚太传统医药,2011,7(9):25-28.CHEN Zhong,LI Junshan,PENG Xinhua.Rapid quantitative analysis of the Baicalin in Liyan Jiedu granules by near infrared diffuse reflectance spectroscopy[J].Asia-Pacific Traditional Medicine,2011,7(9):25-28.
[11]李军山,高晗,张肖建,等.近红外光谱法快速测定猪去氧胆酸含量[J].中国现代中药,2016,18(5):588-590.LI Junshan,GAO Han,ZHANG Xiaojian,et al.Rapid quantitative analysis of hyodeoxycholic acid by near infrared spectroscopy[J].Modern Chinese Medicine,2016,18(5):588-590.
[12]郝磊,李军山,彭新华,等.丹参药材水分近红外定量模型的建立[J].中国药物警戒,2016,13(8):464-467.HAO Lei,LI Junshan,PENG Xinhua,et al.Establishment of rapid analysis of water in Salvia Miltiorrhiza by near infrared diffuse reflectance spectroscopy[J].Chinese Journal of Pharmacovigilance,2016,13(8):464-467.
[13]刘国海,韩蔚强,江辉.基于近红外光谱的橄榄油品质鉴别方法研究[J].光谱学与光谱分析,2016,36(9):2798-2801.LIU Guohai,HAN Weiqiang,JIANG Hui.Study on quality identification of olive oil based on near infrared spectra[J].Spectroscopy and Spectral Analysis,2016,36(9):2798-2801.
[14]YUN Yonghuan,WANG Weiting,TAN Minli,et al.A strategy that iteratively retains informative variables for selecting optimal variable subset in multivariate calibration[J].Analytica Chimica Acta,2014,807(1):36-43.
[15]谢越,周成,涂从,等.近红外光谱技术定量分析连作滁菊土壤中的阿魏酸含量[J].分析化学,2017,45(3):363-368.XIE Yue,ZHOU Cheng,TU Cong,et al.Quantitative determination of ferulic acid content in Chrysanthemum Morifolium cv(Chuju)continuous cropping soil using near infrared spectroscopy[J].Chinese Journal of Analytical Chemistry,2017,45(3):363-368.
[16]乔瑶瑶,赵武奇,胡新中,等.近红外光谱技术检测燕麦中蛋白质含量[J].中国粮油学报,2016,31(8):138-142.QIAO Yaoyao, ZHAOWuqi, HUXinzhong,etal.Determination of protein content in oat using near-infrared spectroscopy[J].Journal of the Chinese Cereals and Oils Association,2016,31(8):138-142.
[17]商志伟,赵云,沈奇,等.紫苏种子品质的近红外光谱分析[J].光谱学与光谱分析,2017,37(12):3719-3724.SHANG Zhiwei,ZHAO Yun,SHEN Qi,et al.Quality analysis with near-infrared spectroscopy in Perilla seed[J].Spectroscopy and Spectral Analysis,2017,37(12):3719-3724.
[18]张金伟,张延莹,刘岩,等.近红外光谱法在线质量监控白芍工业化提取[J].中草药,2011,42(12):2459-2461.ZHANG Jinwei,ZHANG Yanying,LIU Yan,et al.On-line quality control for Paeoniae Radix Alba industrial extraction by NIRS[J].Chinese Traditional and Herbal Drugs,2011,42(12):2459-2461.
[19]李军山,陈钟,彭新华,等.杜仲不同炮制品配方颗粒红外快速鉴别[J]河北工业科技,2016,33(6):503-508.LI Junshan,CHEN Zhong,PENG Xinhua,et al.Rapid identification of different processed products of Eucommia ulmoides formula granules by FTIR[J].Hebei Journal of Industrial Science and Technology,2016,33(6):503-508.