目的:建立在线原位测定多潘立酮片在流化床制粒干燥过程中颗粒水分含量的定量分析模型。 方法:使用微型近红外光谱仪,在线原位收集多潘立酮片制粒干燥过程的近红外光谱,在不同的干燥时间取样以获得不同水分的建模样品,采用一阶导数(FD),多元散射校正(MSC)和Savitzky-Golay卷积平滑的光谱预处理方法,选择1 100~1 600 nm波段,运用偏最小二乘回归建立近红外定量分析模型并进行方法学验证,包括准确度、精密度、专属性、线性和范围、耐用性。结果: 所建模型的交叉验证均方根误差(RMSECV)为0.079 7,决定系数(R2)为0.994 5;预测均方根误差(RMSEP)为0.092 3,R2为0.986 0。方法学验证中各项指标均符合要求。 结论:微型近红外光谱仪应用于在线原位测定多潘立酮片颗粒的含水量是可行的,为过程分析技术在制药行业在线原位的应用提供了实验基础。
Objective: To establish a quantitative model to in-line in situ determination of the water content of domperidone tablets particles in fluidized bed granulation drying process. Methods: Using micro near infrared spectrometer, in-line collected near infrared(NIR) spectrum of domperidone tablets particles in granulation drying process, took sample at different drying time to acquire sample in different level of water content. The pretreatment method of first derivative(FD), multiplicative scatter correction (MSC) and Savitzky-Golay smoothing were selected. The modeling band was 1 100-1 600 nm, model was established by partial least square(PLS) method, and validation was executed including accuracy, precision, specificity, linearity and range, robustness. Results: The root mean square error of cross validation(RMSECV) was 0.079 7,the coefficient of determination(R2) was 0. 994 5,the root mean square error of prediction(RMSEP) was 0.092 3, the R2 was 0.986 0. All validation results met predefined criteria. Conclusion: It is feasible for using micro NIR spectrometer to in-line measure the water content of domperidone tablets particles which provides an experimental basis for the in-line application of process analysis technology in pharmaceutical industry.
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