近红外光谱技术在热毒宁注射液栀子提取液浓缩过程中的应用  

Application of Near-infrared Spectroscopy on Concentration Process of Gardeniae Fructus Extracting Solution from Reduning Injection

作　　者：李云[1,2] 毕宇安[2,3] 王振中[2,3] 萧伟[1,2,3] 

机构地区：[1]南京中医药大学,南京210000 [2]中药制药过程新技术国家重点实验室,江苏连云港222001 [3]江苏康缘药业股份有限公司,江苏连云港222001

出　　处：《中国实验方剂学杂志》2016年第12期1-6,共6页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国家"重大新药创制"科技重大专项(2013ZX09402203)

摘　　要：目的:应用近红外光谱技术(NIR)建立热毒宁注射液栀子提取液浓缩过程中绿原酸和栀子苷质量分数、固含量、密度的快速定量分析模型,实时反映浓缩状态,实现栀子提取液浓缩过程的质量控制。方法:收集栀子提取液浓缩过程中样品,同时采集浓缩过程在线NIR光谱,经过异常点剔除、光谱预处理和波段选择,运用偏最小二乘法(PLS)分别建立NIR光谱与绿原酸和栀子苷质量分数、固含量、密度分析值之间的定量校正模型,并对未知样品进行预测。结果:PLS模型中,绿原酸和栀子苷质量分数、固含量、密度校正集相关系数分别为0.990 5,0.994 3,0.986 2,0.987 9,交叉验证误差均方根分别为0.112,0.368,0.148,0.013;验证集相关系数分别为0.987 2,0.992 5,0.981 6,0.982 3,预测误差均方根分别为0.181,0.302,0.128,0.016,相对预测偏差均<6.0%,能够满足中药生产过程中质量分析要求。结论:该法操作简便、快速无损且准确可靠,可用于热毒宁注射液栀子提取液浓缩过程中绿原酸和栀子苷含量、固含量、密度等质控指标的快速分析及监测。Objective： To truly realize quality control of concentration process of Gardeniae Fructus extracting solution,near-infrared spectroscopy（ NIR） was used to establish a rapid quantitative analysis model for contents of chlorogenic acid and geniposide, total solid content and density during concentrating process of Gardeniae Fructus extracting solution,which could real-timely reflect its state. Method： Concentration solution samples of Gardeniae Fructus extracting solution in the workshop were collected and on-line NIR were acquired simultaneously. After rejection of abnormal samples,pretreatment of spectra and choice of the corresponding wave band,the multivariate calibration models were respectively established using partial least square method（ PLS）between spectra and chlorogenic acid content, geniposide content, total solid content and density, then these models were measured by reference method, which could be used to predicte unknown samples. Result：Correlation coefficients of contents of chlorogenic acid and geniposide,total solid content and density in calibration set were 0. 990 5,0. 994 3,0. 986 2 and 0. 987 9; correlation coefficients in validation set were 0. 987 2,0. 992 5,0. 981 6 and 0. 982 3; root mean square errors of cross-valibration（ RMSECV） were 0. 112,0. 368,0. 148 and 0. 013, root mean square error of prediction（ RMSEP） were 0. 181,0. 302,0. 128 and 0. 016,respectively. Relative standard errors of predictions（ RSEP） were lower than 6. 0%,which can satisfy the quality control standard in production process of traditional Chinese medicine. Conclusion： The method is simple,accurate,reliable and applicable for fast analysis and monitoring of contents of chlorogenic acid and geniposide,total solid content and density in concentration process of Gardeniae Fructus extracting solution from Reduning injection.

关 键 词：近红外光谱 热毒宁注射液 栀子 浓缩液 绿原酸 

分 类 号：R283.6[医药卫生—中药学] O433.4[医药卫生—中医学]