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声光可调-近红外光谱法快速判断精芪双参胶囊的混合终点及测定黄芪甲苷的含量
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篇名: 声光可调-近红外光谱法快速判断精芪双参胶囊的混合终点及测定黄芪甲苷的含量
TITLE:
摘要: 目的:建立快速判断精芪双参胶囊的混合终点及测定黄芪甲苷含量的方法。方法:采用声光可调-近红外光谱法(AOTF-NIR)结合主成分分析法及移动窗标准偏差法判断混合终点;以一阶导数法联合平滑滤波系数法预处理混合终点样品光谱,并采用偏最小二乘法建立混合终点样品中黄芪甲苷含量的定量模型,并采用高效液相色谱-蒸发光散射检测法(HPLC-ELSD)测定混合终点样品中黄芪甲苷的含量以进行验证。结果:混合终点样品中黄芪甲苷含量测定方法学经验证符合要求。混合物料样品在混合30 min时可达到混合终点,NIR预测结果与HPLC-ELSD法实测的混合终点结果一致;定量模型的主成分维数为9,决定系数为0.954 9,校正均方根偏差为0.039 2,预测均方根偏差为0.042 6;黄芪甲苷含量的NIR预测平均值为11.74 mg/g,HPLC-ELSD法实测平均值为11.38 mg/g,平均偏差为3.16%。结论:AOTF-NIR法可快速判断精芪双参胶囊的混合终点,并能够快速测定混合终点样品中黄芪甲苷的含量,可提高其混合过程的质量控制水平,缩短混合周期。
ABSTRACT: OBJECTIVE: To establish the method for rapid judgement of blending endpoint of Jingqi shuangshen capsules and content determination of astragaloside Ⅳ. METHODS: AOTF-NIR combined with principal component analysis and Moving Block Standard Deviation method was used to identify the blending endpoint. First derivative combined with savitzky-golay filter method were used to spectrum pretreatment. The partial least square method was used to establish quantitative analysis model of the content of astragaloside Ⅳin mixed endpoint sample. The content of astragaloside Ⅳ in mixed endpoint sample was determined by HPLC-ELSD to validate the model. RESULTS: Methodology validation of content determination of astragaloside Ⅳ in mixed material sample and mixed endpoint sample was in line with the requirements. NIR monitoring results showed that the product reached the blending endpoint after 30 min. The results of NIR monitoring were generally consistent with the results of HPLC-ELSD. The principal component dimension of the quantitative model was 9; determination coefficients was 0.954 9; Root Mean Square of Calibration of the model was 0.039 2; Root Mean Square Error of Prediction of the model was 0.042 6. Predicted average value of astragaloside Ⅳ by NIR was 11.74 mg/g, and measured average value of astragaloside Ⅳ by HPLC-ELSD was 11.38 mg/g; average deviation was 3.16%. CONCLUSIONS: AOTF-NIR can rapidly judge the blending endpoint sample of Jingqi shuangshen capsules, rapidly determine the content of astragalosideⅣin mixed endpoint material, improve the quality control level of blending process and shorten blending cycle.
期刊: 2018年第29卷第12期
编辑: 苏婷,姜文月,李亚东,任绪华,马子君,齐美欣,崔宪利,高陆
AUTHORS: SU Ting,JIANG Wenyue,LI Yadong,REN Xuhua,MA Zijun,QI Meixin,CUI Xianli,GAO Lu
关键字: 声光可调-近红外光谱法;移动窗标准偏差法;一阶导数法;平滑滤波系数法;偏最小二乘法;精芪双参胶囊;混合终点;黄芪甲苷
KEYWORDS: AOTF-NIR; Moving Block Standard Deviation method; First derivative method; Savitzky-golay filter method; Partial least square method; Jingqi shuangshen capsules; Blending endpoint; Astragaloside Ⅳ
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