利用NIRS技术快速测定制何首乌中游离蒽醌含量

Rapid content determination of free anthraquinones in Polygoni Multiflori Radix Praeparata by using NIRS

目的:建立测定制何首乌中游离蒽醌含量的近红外光谱(NIRS)分析模型,实现利用NIRS技术快速测定制何首乌中游离蒽醌含量。方法:采用HPLC法测定制何首乌中游离蒽醌的含量,利用近红外光谱仪采集制何首乌样品的近红外原始光谱,分辨率为8 cm^(-1),扫描64次,扫描范围为12 000~4 000 cm^(-1),温度(22±0.5)℃;相对湿度25%~35%。用TQ 8.0分析软件联合样品游离蒽醌含量数据与近红外光谱,经化学计量学方法对原始光谱进行预处理后,选择合适波段和最佳主因子数后,以PLS法建立近红外光谱分析模型。结果:经对比分析,采用多元散射矫正(MSC)+一阶导数(first derivative)法对近红外光谱进行预处理,以4 200~5 000和5 230~9 870 cm^(-1)为建模波段,8为最佳主因子数,结合PLS法建立了测定制何首乌中游离蒽醌含量的近红外光谱分析模型。所建模型的内部交叉验证系数R2=0.990 52、RMSEC=0.014 2、RMSEP=0.016 0。结论:所建立的模型性能良好,通过采集样品的近红外光谱信息,即可实现准确、快速地测定制何首乌中游离蒽醌的含量,所用物理检测技术可应用于生产加工在线监测。

Objective： To establish a near-infrared reflectance spectroscopy （NIRS） analysis model for measuring the content of free anthraquinones in Polygoni Multiflori Radix Praeparata, so as to realize the rapid measurement of anthraquinone in Radix Polygoni Multiflori.Methods： HPLC was used to determine the concentration of free anthraquinones in Polygoni Multiflori Radix Praeparata, and the near infrared spectrums were gathered by NIRS.The resolution was 8 cm-1.The spectrums were scanned for 64 times, the scanning range was 12 000-4 000 cm-1, the temperature was （22±0.5）℃, and the relative humidity was 25%-35%.Then, TQ 8.0 analystical software was used to combine the HPLC data with the near infrared spectrums.After preprocessing the near infrared spectrums by chemometrics, the appropriate bands and the best principal factors were selected and the near infrared spectroscopy analysis model was established by PLS method.Results： In this work, the chemometric method of SNV＋First derivative was used to preprocess the infrared spectrums.Based on PLS algorithm, the NIRS analysis model was established, which of the optimal wavelength intervals were 4 200-5 000 and 5 230-9 870 cm-1, and 8 was the best principal factor number.The correlation coefficients （R2）, the root-mean-square error of calibration （RMSEC） and the root-mean-square error of predication （RMSCP） of the calibration model were 0.990 52, 0.014 2, and 0.016 0, respectively.Conclusion： The NIRS calibration model has a high quality, and it can be used in measuring the content of free anthraquinones in Polygoni Multiflori Radix Praeparata.