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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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(AOTFNIR)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。
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 HPLCELSD 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.
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 HPLCELSD 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.
引文
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[12]吴莎,刘启安,李云,等.最小二乘支持向量机和偏最小二乘法在栀子中间体纯化工艺近红外定量分析中的应用[J].中草药,2015,46(7):990-997.
[13]周昭露,李杰,黄生权,等.近红外光谱技术在中药质量控制应用中的化学计量学建模:综述和展望[J].化工进展,2016,35(6):1627-1645.
[2]陈红英,李琼娅,陈佳乐,等.近红外光谱技术用于正天丸混合过程终点的判断[J].中国实验方剂学杂志,2016,22(12):13-16.
[3]安红,史新元,温建省.便携式近红外漫反射中药质量监控仪的研制[J].光学技术,2007,33(S1):343-344.
[4]何智慧,练文柳,吴名剑,等.声光可调-近红外光谱技术分析烟草主要化学成分[J].分析化学,2006,34(5):702-704.
[5]薛忠,徐冰,张志强,等.药物粉末混合过程在线监控技术研究进展[J].中国药学杂志,2016,51(2):91-95.
[6]丁海樱,金叶,刘雪松,等.中药粉末混合过程近红外在线检测研究[J].中国药学杂志,2013,48(14):1151-1156.
[7]周鹏,胡明勋,李浩飞,等.不同品种、产地和种植方式黄芪药材中黄酮类成分的质量分析[J].中国药房,2016,27(18):2575-2578.
[8]钟英杰,李亮,庞云露,等.近红外光谱技术在中药研究中的应用[J].药物分析杂志,2015,35(10):1697-1703.
[9]金叶,杨凯,陈木洲,等.微型近红外仪用于众生丸粉末混合过程的在线监测研究[J].中国中药杂志,2011,36(21):2963-2966.
[10]黄丽丽,朱健萍.近红外漫反射光谱法测定谷维素片的含量[J].中国药房,2016,27(36):5132-5134.
[11]谢彩侠,谢惠英,白雁,等.近红外光谱法快速测定知母中芒果苷的含量[J].中国实验方剂学杂志,2015,21(10):59-62.
[12]吴莎,刘启安,李云,等.最小二乘支持向量机和偏最小二乘法在栀子中间体纯化工艺近红外定量分析中的应用[J].中草药,2015,46(7):990-997.
[13]周昭露,李杰,黄生权,等.近红外光谱技术在中药质量控制应用中的化学计量学建模:综述和展望[J].化工进展,2016,35(6):1627-1645.