作　　者： (）;

机构地区： 广东药科大学中药学院

出　　处： 《中国实验方剂学杂志》 2018年第7期27-32,共6页

摘　　要： 目的：醋香附的含量测定采用挥发油测定法，检测耗时长、操作复杂，且未规定具体有效成分及其含量评价指标。为解决此问题，探索采用先进的检测技术测定醋香附中具体有效成分的含量，结合近红外光谱技术，建立快速、准确的定量分析模型。方法：采用HPLC检测α-香附酮的含量，流动相甲醇（A）-0．1％磷酸水溶液（B）梯度洗脱（0～10min，30％～73％A；10-40min，73％～76％A；40～50min，76％～30％A），检测波长252nm；采用近红外光谱仪采集醋香附的近红外光谱图，以醋香附中α-香附酮的HPLC测量值为参考，建立偏最小二乘法（PLS）定量分析模型。结果：建立了α-香附酮定量模型，模型的内部交叉验证系数（R^2），校正均方差（RMSEC），预测均方差（RMSEP）分别为0．9875，0．0062，0．0072，交叉验证均方差（RMSECV）为0．0204，经验证模型平均回收率101．33％。结论：该方法检测速度快、预测结果准确，可用于快速测定醋香附中α-香附酮的含量。 Objective： Distillation method was employed to determine content of Cyperi Rhizoma stir- fried with vinegar, which had features of wasting time, complex operation, without specific effective component content index in the quality standard. In order to solve these problems, this study was to explore the method for determination of specific active ingredients in Cyperi Rhizoma stir-fried with vinegar by advanced detection technology, combined with near-infrared spectroscopy, to establish a rapid and accurate quantitative analysis model. Method： HPLC was adopted to determine the content of c^-cyperone with mobile phase of methanol-0. 1% phosphoric acid for gradient elution and detection wavelength at 252 nm. The near infrared spectra of Cyperi Rhizoma stir-fried with vinegar were collected by near-infrared spectrometer. Taking HPLC measured value as a reference, partial least squares （PLS） was used to establish the quantitative model of c^-cyperone. Result： The quantitative model of c^-cyperone was established, the correlation coefficient of calibration （R2） , root-mean-square error of calibration （RMSEC） and root-mean-square error of prediction （RMSEP） of the calibration model were O. 987 5, 0. 006 2 and 0. 007 2; the root-mean-square error of cross-validation （RMSECV） of the calibration model was 0. 020 4, the average recovery was 101.33%. Conclusion： The method has fast detection speed and accurate prediction results, it can be applied to quickly determine the content of a-cyperone in Cyperi Rhizoma stir-fried with vinegar.

关 键 词： 近红外光谱技术 醋香附 香附酮 定量模型 偏最小二乘法 预测均方差 一阶导数

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