傅里叶红外光谱结合HPLC对不同产地南葶苈子成分的含量测定

Content Determination of Different Regions Nantinglizi(Descurainia sophia)by NIRS and HPLC

目的创建一种能够快速测定南葶苈子药材中芥子碱硫氰酸盐(sinapine thiocyanate,SH),槲皮素-3-O-β-D-葡萄糖-7-0-β-D-龙胆双糖苷(quercetin-3-O-beta-D-glucose-7-O-beta-D-gentiobioside,QGG),异鼠李素-3-O-β-D-吡喃葡萄糖苷(isorhamnetin-3-O-glucoside,IG),槲皮素-3-O-β-D-吡喃葡萄糖苷(quercetin3-O-β-D-glucopyranoside,QG)4种成分的方法。方法高效液相色谱法(high performance liquid chromatography,HPLC)测定南葶苈子样品中SH、QGG、IG、QG的含量,采用偏最小二乘法(partial least squares method,PLS)建立南葶苈子中SH、QGG、IG、QG的定量分析模型。结果所创建的QGG、QG、IG、SH的定量分析模型的内部交叉验证决定系数(R2)分别为0.9270、0.9266、0.8086、0.8289;校正均方差(root mean square error of calibration,RMSEC)分别为0.0100、0.00263、0.00313、0.111;验证均方差(root mean square error of prediction,RMSEP)分别为0.0139、0.00715、0.00395、0.0860。其中SH的特征光谱为9100~6100 cm-1;QGG的特征光谱为7300~5500 cm-1;IG的特征光谱为9500~6700 cm-1;QG的特征光谱为8200~5100 cm-1。结论利用傅里叶红外光谱建立的定量模型,能够对南葶苈子药材中QGG、QG、IG、SH的含量进行无损测定。此外通过近红外光谱PCA分析发现道地产地南葶苈子与非道地产地南葶苈子的差异较大,道地产地南葶苈子之间的差异较小。

Objective To establish a rapid method for simultaneous determination of quercetin 3-O-β-D-glucose-7-O-β-D-gentiandioside(QGG),quercetin3-O-β-D-glucopyranoside(QG),isorhamnetin3-O-β-D-glucopyranoside(IG)and sinapine thiocyanate(SH)in Nantinglizi(Descurainia sophia).Methods The contents of QGG,QG and IG and sinapine thiocyanate in Nantinglizi(Descurainia sophia)were determined by HPLC.Partial least squares method(PLS)was used to establish the quantitative analysis model of QGG,QG,IG and sinapine thiocyanate in the samples measured by HPLC.Results The internal cross validation determination coefficients(R2)of the established quantitative analysis models for QGG,QG,IG and sinapine thiocyanate were 0.9270,0.9266,0.8086 and 0.8289,respectively.The Root Mean Square Errors of Calibration(RMSEC)were 0.0100,0.00263,0.00313 and 0.111,respectively.The Root Mean Square Errors of Prediction(RMSEP)were 0.0139,0.00715,0.00395 and 0.0860,respectively.The characteristic spectrum of sinapine thiocyanate ranged from 9100 to 6100 cm-1.The characteristic spectrum of QGG was 7300~5500 cm-1.The characteristic spectrum of IG ranged from 9500 to 6700 cm-1.The characteristic spectrum of QG was 8200~5100 cm-1.Conclusion The quantitative analysis model established by NIR spectroscopy can be used for rapid and nondestructive determination of QGG,QG,IG and sinapine thiocyanate in Nantinglizi(Descurainia sophia).In addition,PCA analysis showed that there were significant differences between traditional and non-traditional regions in Nantinglizi(Descurainia sophia).But there are less differences in traditional regions.