药渣粒径对中药提取过程在线检测取样系统影响的模拟研究  

A Simulation Study for Effect of Particle Size on On-line Measurement Sampling System of Traditional Chinese Medicine Extraction Process

作　　者：隋丞琳[1] 林兆洲[1] 吴志生[1] 徐冰[1] 李洋[1] 史新元[1] 乔延江[1] 

机构地区：[1]北京中医药大学中药信息工程研究中心,北京100102

出　　处：《分析化学》2013年第12期1899-1904,共6页Chinese Journal of Analytical Chemistry

基　　金：国家"重大新药创制"科技重大专项(No.2010ZX09502-002)资助

摘　　要：以栀子提取液为研究载体,采用离线方式采集经不同孔径滤网过滤后样品的近红外光谱,并以高效液相测定值为参考值,采用偏最小二乘算法建立栀子苷定量校正模型,探讨基于中药提取过程的在线检测旁路预处理系统可靠性及预处理系统中滤器孔径大小对所建立定量校正模型的影响。结果表明,提取液经筛分滤过后样品与原提取液样品经配对t检验,验证同一样品经过滤后所含栀子苷浓度无显著性差异,可以代表原液样品进行数据分析,进一步证明旁路预处理系统可用于在线检测的可行性。经300目标准筛过滤后的样品以原始光谱建立的定量模型预测能力最好(校正集的交叉验证均方差RMSECV=0.1962,预测均方差RMSEP=0.1867,系统偏差Bias=0.0256)。通过实践明确取样系统的可行性,合理选择预处理系统滤器孔径,能够有效改善并提高所建模型预测能力,解决中药提取在线过程分析应用技术难题。As the objective of simulation study, the samples of gardenia fructus extract were collected every 5 min while boiling for 60 rain. Each sample was filtrated by different sizes of sieve meshes, and then scanned by the near infrared spectra. Using the HPLC determined value for reference, quantitative calibration models of geniposide were established by the partial least square method. Based on on-line near infrared spectral technology, the effects of by-pass preprocess system and filter mesh on the accuracy of calibration model were further studied. By the analysis of paired t test, the filtrated sample was compared with original extract, which illustrated that the filtrated sample and the original extract weren＇t significant different, so the sample after filtration could be representative of the original gardenia fructus extract for the data analysis. In addition, after the sample was filtrated by a sieve with meshes size of 0. 049 ram, quantitative prediction model, which was built by raw spectrum pretreatment, could reach the ideal prediction result （ Root Mean Square Error of Cross Validation （RMSECV） was 0. 1962, Root Mean Square Error of Prediction （RMSEP） was 0. 1867, Bias was 0. 0256）. It was recommended that proper size of sieve mesh could be selected by the simulation study, and then the feasibility of sample pretreatment system could be verified on-line, finally the stable preprocess system could be established. These steps could improve the performance of prediction models dramatically.

关 键 词：中药 近红外光谱 提取过程 在线检测 取样系统 

分 类 号：TQ460.72[医药卫生—药物分析学]