[关键词]
[摘要]
目的 应用近红外光谱(NIRS)技术结合偏最小二乘法(PLS)建立当归中多指标成分的快速无损检测方法,以更好地控制当归药材和饮片的质量。方法 采集购买不同产地的当归样品共108批。建立同时测定当归中7种成分含量的超高效液相色谱(UPLC)方法,并以其测定值为参比;以积分球漫反射模式采集当归样品的NIRS图;采用PLS等化学计量学手段建立各指标性成分的参比值与NIRS图的定量校正模型。分别对建模过程的各个阶段进行优化,包括样本集的选择、不同预处理方法和不同光谱区段的选择。结果 所建立的绿原酸、阿魏酸、异绿原酸A、藁本内酯、丁烯基苯肽、洋川芎内酯I和欧当归内酯A的模型校正集相关系数分别为0.937 6、0.970 2、0.963 4、0.991 1、0.962 4、0.966 6和0.947 6;预测均方差分别为0.072 1、0.038 9、0.011 3、0.483 0、0.017 5、0.178 0和0.097 0。NIRS模型预测值与UPLC测定值具有良好的线性相关关系,模型预测效果良好。结论 采用NIRS技术结合PLS可以快速对当归中绿原酸、阿魏酸、异绿原酸A、藁本内酯、丁烯基苯肽、洋川芎内酯I和欧当归内酯A 7种成分的含量进行检测,方法操作简便、结果可靠。
[Key word]
[Abstract]
Objective To established a rapid nondestructive determination method for the multi-marker constituents in Angelica sinensis by near infrared spectroscopy (NIRS) combined with the partial least squares (PLS) method in order to improve the quality control for A. sinensis. Methods A total of 108 batches of A. sinensis from different origins were collected for the research. An Ultra performance liquid chromatography (UPLC) method was established to measure the content of the seven components in A. sinensis, which were adopted as the reference value. And the integrating sphere diffuse reflection mode was employed to collect the NIR spectrum. The quantitative calibration model between the near infrared spectrum and the reference content of each component to be measured was established by PLS and other chemometrics methods. Each part of the modeling process was optimized respectively, including the selection of calibration set and validation set, different pretreatment methods and different spectral section. Results The correlation coefficient for calibration set of chlorogenic acid, ferulic acid, isochlorogenic acid A, ligustilide, butylidenephthalide, senkyunolide I and levistilide A were 0.937 6, 0.970 2, 0.963 4, 0.991 1, 0.962 4, 0.966 6 and 0.947 6, respectively; The root mean square error of prediction (RMSEP) were 0.072 1, 0.038 9, 0.011 3, 0.483 0, 0.017 5, 0.178 0 and 0.097 0, respectively. The predicted values of NIRS models and the measured values of UPLC showed a good linear relation, which presented a great prediction ability of the models. Conclusion The methods of NIRS combined with PLS can be applied for the rapid content determination of seven components in A. sinensis including chlorogenic acid, ferulic acid, isochlorogenic acid A, ligustilide, butylidenephthalide, senkyunolide I and levistilide A, which is proved to be simple and reliable.
[中图分类号]
[基金项目]
国家中医药行业科研专项资助(201407003)