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 statistical 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
Keywords
Near infrared diffuse reflectance spectrophotometryShouwu pillsStilbene glycosideContentPartial least square method