基于近红外光谱技术对双黄连口服液中黄芩苷、绿原酸和连翘苷进行现场快速定量分析方法的研究

Research based on near infrared spectroscopy on-site rapid quantitative analysis method for baicalin,chlorogenic acid and forsythin in Shuanghuanglian oral liquid

目的:建立应用声光可调滤光器(AOTF)-近红外(NIR)光谱技术对双黄连口服液进行现场快速定量分析的方法。方法:收集7个厂家58个不同批号双黄连口服液为样本,利用HPLC法测定校正集样品中3个成分的含量,并进行方法学考察,继而选用便携式AOTF近红外光谱仪采集光谱,通过The Unscrambler分析软件,利用偏最小二乘法(PLS1)对双黄连口服液中黄芩苷、绿原酸和连翘苷3个指标成分分别建立了定量分析模型,并对模型的微分处理方法、波长范围进行了研究。结果:建立的定量分析模型具有较好的预测能力,验证集样品3个成分黄芩苷、绿原酸和连翘苷的NIR预测值与HPLC参考值间的相关系数(r)分别为0.9909,0.9913,0.9640;平均相对误差分别为0.96%,5.62%,2.75%。方法精密度RSD值(n=20)分别为0.86%,0.82%,0.73%;方法稳定性RSD值(n=9)分别为0.98%,1.2%,1.1%。结论:本研究使用便携式AOTF近红外光谱仪,利用化学计量学软件,所建立的对双黄连口服液中3个指标成分的分析方法快速、准确,为双黄连口服液的现场、即时快速定量分析提供了一种新方法,同时也为生产过程中的在线质量监控奠定了基础。

Objective：To establish a new method for on-site rapidly analyzing the Chinese formulated product Shuanghuanglian oral liquid by portable acousto-optic tunable filter （AOTF）-near infrared（NIR） spectroscopy.Methods：58 different batches of Shuanghuanglian oral liquid collected fromseven pharmaceutical factories were usedto test.Three components in calibration set samples were examined by HPLC.Then,a portable fifth generation AOTF-NIR spectrometer was used to analyze the samples by the unscrambler program. Quantitative analysis models of three index constituents,which are baicalin,chlorogenic acid,and forsythin in Shuanghuanglian oral liquid,are estab-lished respectively take advantage of partial least squares（PLS1）.Conditions for optimal model construction,such as different spectral pretreatments and wavelength regression,were studied within the framework of the unscrambler program.Results：The quantitative analysis models performed well for prediction,with the correlation coefficients for the three analyzed ingredients equal to0.9909,0.9913,and 0.9640,respectively.The average relative errors for the test sets were 0.96%,5.62%,and 2.75%,respectively.The precision RSDs（n=20）were 0.86%,0.82%,0.73%,and the stability RSDs（n=9）were 0.98%,1.2%,1.1%,respectively.Conclusion：The analysis method based on AOTF-NIR spectroscopy provides a foundation for rapid quantitative analyses of Shuanghuanglian oral liquid,which sets up the foundation of product-line control of Shuanghuanglian oral liquid and can be used for on-site rapid screening of drugs.