近红外特征谱段相关系数法测定中药胶囊中添加枸橼酸西地那非  

Near Infrared Correlation Coefficient Method with Characteristic Spectral Band for the Determination of Illegal Addition of Sildenafil Citrate in Capsules of Chinese Traditional Medicine

作　　者：王学良[1,2] 冯艳春[1] 胡昌勤[1] 

机构地区：[1]中国药品生物制品检定所,北京100050 [2]新疆维吾尔自治区食品药品检验所,乌鲁木齐830000

出　　处：《分析化学》2009年第12期1825-1828,共4页Chinese Journal of Analytical Chemistry

基　　金：国家科技支撑计划(No.2008BA155B06)资助项目

摘　　要：利用近红外特征谱段相关系数法对中药胶囊中是否添加枸橼酸西地那非进行快速定性分析。分别使用近红外光谱仪的积分球和光纤附件测定光谱,以枸橼酸西地那非化学对照品的近红外光谱为参照光谱,选择特定谱段,根据枸橼酸西地那非被掺入胶囊中的最小起效浓度建立待测样品光谱与参照光谱在该谱段的相似系数阈值,定性判断待测样品是否含有枸橼酸西地那非。积分球方法:选择6070～5800 cm-1和4170～4070 cm-1谱段,阈值为70%,用79个含枸橼酸西地那非的市售样品验证该方法,相关系数大于70%的有72个,占样品总量的91.14%;光纤方法:选定6070～5800 cm-1谱段为特征谱段,设定阈值为65%,用247个含枸橼酸西地那非的市售样品进行验证,相关系数大于65%的有216个,占样品总量的87.45%。实验证明此方法具有较好的预测能力,可作为市场上该种非法添加药物的快速有效检查手段。A near infrared （NIR） method for the detection of illegal addition of sildenafil citrate in capsules of Chinese traditional medicine was constructed. The diffuse reflectance near infrared spectra were recorded using integrated sphere and fiber optics respectively. Using the spectra of the sildenafil citrate standard as reference spectra, the threshold of the correlation coefficient was set up based on the minimum effective concen- tration of the sildenafil citrate. By comparing the threshold with the correlation coefficient between the tested spectra and the reference spectra in the selected spectral range, the tested sample contains sildenafil citrate is determined. For the integrated sphere method, the spectral range of 6070-5800cm^-1 and 4170-4070 cm^-1 were selected, and 70% was set as threshold. For the fiber method, 6070-5800cm^-1 and 65% were used. 79 and 247 batches of the Chinese traditional medicines contained sildenafil citrate collected from the Chinese market were used to validate the two methods separately. The accuracy of the integrated sphere method was 91.14%, and that of fiber method was 87.45%.

关 键 词：近红外漫反射光谱 相关系数法 定性分析 中药非法添加 枸橼酸西地那非 

分 类 号：R286[医药卫生—中药学]