近红外定性模型结合HPLC指纹图谱评价川芎饮片的质量

Quality evaluation of Chuanxiong Rhizoma based on near infrared qualitative model combined with HPLC fingerprint

目的建立川芎饮片的HPLC指纹图谱,并建立川芎饮片的近红外光谱(NIR)定性及定量模型。方法采用ZORBA SB-C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-1%冰乙酸溶液,梯度洗脱,柱温35℃,进样量5μL,指纹图谱检测波长为280 nm、流速1.0 mL·min^(-1),含量测定检测波长为320 nm、流速1.2 mL·min^(-1)。利用傅里叶近红外光谱仪采集川芎样品的NIR数据。采用相似度评价、聚类分析对37批川芎样品的指纹图谱进行研究,并将最终聚类的结果导入近红外TQ软件,采用马氏距离法进行NIR定性建模;将阿魏酸和藁本内酯的含量数据导入近红外TQ软件,采用PLS法分别建立阿魏酸和藁本内酯的NIR定量模型。结果以NIR定性模型归属于A类,且定量模型预测阿魏酸含量>0.5%、藁本内酯含量大于2%为一等品;以归属于B类,且阿魏酸含量≥0.3%、藁本内酯含量≥1.5%为二等品;以归属于C类,且阿魏酸≥0.1%、藁本内酯含量≥1%为三等品。结论初步建立了基于指纹图谱技术和指标性成分含量的川芎饮片的质量评价方法,建立的NIR定性模型结合阿魏酸、藁本内酯的NIR定量模型可实现川芎饮片质量的快速评价。

OBJECTIVE To establish an HPLC fingerprint of Chuanxiong Rhizoma,and to establish qualitative and quantitative models of near infrared spectroscopy(NIR)for the quality evaluation of Chuanxiong Rhizoma.METHODS ZORBA SB-C_(18)(250 mm×4.6 mm,5μm)column was used,and the Methanol-1%glacial acetic acid solution was used as mobile phase with gradient elution.The column temperature was 35℃,and injection volume was 5μL.The detection wavelength of fingerprint was 280 nm with a flow rate of 1.0 mL·min^(-1).The detection wavelength of content determination was 320 nm with a flow rate of 1.2 mL·min^(-1).The NIR data of Chuanxiong Rhizoma were collected by Fourier near infrared spectrometer.Similarity evaluation and cluster analysis were used to study the fingerprints of 37 batches of Chuanxiong Rhizoma samples,and the final clustering results were imported into near infrared TQ software,and the NIR qualitative modeling was carried out by Mahalanobis distance method.The contents of ferulic acid and ligustilide were imported into near infrared TQ software,and the NIR quantitative models of ferulic acid and ligustilide were established by PLS method.RESULTS It was classified as first-class product(class A)according to the NIR qualitative model,with the content of ferulic acid more than 0.5%and ligustilide more than 2%.It was classified as second-class product(class B)with the content of ferulic acid no less than 0.3%and ligustilide no less than 1.5%.It was classified as third-class product(class C)with the content of ferulic acid no less than 0.1%and ligustilide no less than 1%.CONCLUSION The quality evaluation method of Chuanxiong Rhizoma decoction pieces based on fingerprint technology and index component content is preliminarily established.The established NIR qualitative model combined with ferulic acid and ligustilide NIR quantitative model can realize the rapid evaluation of Chuanxiong Rhizoma decoction pieces quality.