近红外漫反射光谱法快速测定首乌丸中二苯乙烯苷的含量  

Rapid Determination of Stilbene Glycoside in Shouwu Pills by Near Infrared Diffuse Reflectance Spectrophotometry

作　　者：刘喜乐[1] 贾灿潮 姬生国[1] 

机构地区：[1]广东药科大学中药学院,广州510006

出　　处：《中国药房》2017年第18期2539-2542,共4页China Pharmacy

基　　金：广东省科技计划项目(No.2009B030801044)

摘　　要：目的:建立快速测定首乌丸中二苯乙烯苷含量的方法。方法:采用高效液相色谱法(HPLC)测定首乌丸中二苯乙烯苷的含量(作为实测值):色谱柱为ODS-C_18,流动相为乙腈-水(25∶75,V/V),流速为0.8 m L/min,检测波长为320 nm,柱温为30℃,进样量为10μL。采用偏最小二乘法-近红外漫反射光谱法建立预测首乌丸中二苯乙烯苷含量的定量校正模型:根据实测值,采集校正集样品76份、验证集样品18份,以标准归一化法、一阶导数法联合滤波法预处理光谱,最佳波段为9 000~4 150 cm^(-1),主成分因子数为12。结果:首乌丸中二苯乙烯苷的含量测定方法学考察符合要求。二苯乙烯苷含量预测的定量校正模型内部交叉验证决定系数为0.991 90,校正均方根偏差为0.020 1,预测均方根偏差为0.023 6,交叉验证均方根偏差为0.076 29,预测值与实测值差异无统计学意义(P>0.05)。结论:该方法准确、稳定、简便,可用于首乌丸中二苯乙烯苷含量的快速测定。OBJECTIVE： To establish the method for the rapid determination of stilbene glycoside in Shouwu pills. METHODS： HPLC method was used to determine the content of stilbene glycoside in Shouwu pills （as measured value）. The determination was performed on ODS-C18 column with mobile phase consisted of acetonitrile-water （25：75, V/V） at the flow rate of 0.8 mL/ min. The detection wavelength was set at 320 nm, and the column temperature was 30℃. The sample size was 10 μL. The partial least square method-near infrared diffuse reflectance spectrophotometry was used to establish quantitative calibration model for predicting the content of stilbene glycoside in Shouwu pills. According to measured value, 76 calibration set samples and 24 validation set samples were collected. Standard normalization method and first-order derivative method combined with Savitzky-Goly filter method were used for spectrum pretreatment. The optimal band ranged 9 000-4 150 cm^-1, and main component factor was 12. RESULTS： The content determination method of stilbene glycoside in Shouwu pills was in line with the requirements. The correlation coefficients, the root-mean-square error of calibration, the root-mean-square error of predication and the root-mean-square error of cross-validation （RMSECV） of the quantitative calibration model were 0.991 90, 0.020 1, 0.023 6 and 0.076 29. There was no sta- tistical significance between predicted value and measured value （P〉0.05）. CONCLUSIONS： The method is accurate, stable and simple, and can be used for rapid determination of stilbene glycoside in Shouwu pills.

关 键 词：近红外漫反射光谱法 首乌丸 二苯乙烯苷 含量 偏最小二乘法 

分 类 号：R917[医药卫生—药物分析学]