注射用单磷酸阿糖腺苷近红外快速定量方法的建立

目的：采用近红外光谱分析技术结合化学计量学建立注射用单磷酸阿糖腺苷快速定量分析方法。方法：以17个厂家生产的133批注射用单磷酸阿糖腺苷为分析对象，其中68批作为校正集，含量范围为46.79%~97.25%；65批作为验证集，含量范围为47.89%~94.49%。首先采集样品的近红外漫反射光谱，同时按法定标准测定样品含量，最后采用偏最小二乘法建立定量模型。结果：采用外部验证建立模型。建模谱段为7 502.3~6 098.2 cm^-1和5 450.2~4 597.8 cm^-1；预处理方法为一阶导数及多元散射校正；维数为7；内部交叉验证决定系数为96.82%，均方根误差为2.64%；外部验证决定系数为97.54%；均方根误差为2.29%。结论：所建立的定量模型可对注射用单磷酸阿糖腺苷进行准确、快速定量分析，绿色，环保，可用于药品的快速分析和检验。

Objective: To develop a quantitative method for quick determination of vidarabine monophosphate for injection by near infrared diffuse reflection spectroscopy technology and chemometrics.Methods: A total of 135 batches of vidarabine monophosphate for injection from 17 different manufactures were enrolled for analysis, among which, 68 batches weres used as the calibration set with the active pharmaceutical ingredient(API)from 46.79%-97.25%, and 65 batches were used as the validation set with the API from 47.89%-94.49%. Firstly, the near infrared diffuse reflection spectrum of the samples were collected. Secondly, the API contents by official method were determined. Finally, the model with the partial least square(PLS)algorithm available in the Quant 2 was developed.Results: Our model was established based on test set validation. The spectra ranges were 7 502.3-6 098.2 cm^-1 & 5 450.2-4 597.8 cm^-1; the pretreatment method was first derivative & multiplicative scattering correction; the rank was 7. In the cross validation, the values of R² and RMSECV were 96.82% and 2.64%, respectively. In the test set validation, the values of R² and RMSEP were 97.54% and 2.29%, respectively.Conclusion: The quantitative model built in this study can analyze the vidarabine monophosphate for injection accurately, quickly, greenly and environmentally-friendly.

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