近红外透射光谱法快速测定布洛芬缓释胶囊释放度

目的: 利用近红外透射光谱分析技术和化学计量学方法对布洛芬缓释胶囊释放度进行快速定量分析。 方法: 以30批布洛芬缓释胶囊为分析对象,首先用近红外透射光谱法采集不同时间段释放液的近红外透射光谱,并以高效液相色谱法测定其含量,最后采用偏最小二乘法建立释放度定量测定模型。 结果: 30批布洛芬缓释胶囊释放度实验得到101个样品数据,采用外部验证建立模型。根据自动分离原理,从101个样品数据中选择了61个数据作为校正集样本,含量范围为4.97%~30.89%;剩余40个数据作为验证集样本,含量范围为5.07%~30.34%;建模谱段为8937~7487 cm^-1及6102~5446 cm^-1;预处理方法为一阶导加多元散射校正;维数为6;内部验证及外部验证的相关系数分别为95.04%和94.37%;内部交叉验证及外部验证均方根误差分别为1.96%和2.04%。 结论: 所建立的释放度快速分析定量模型可对布洛芬制剂进行准确、快速定量分析,方法快速简便,可用于药品的快速分析和检验。

Objective: To quantitatively analyze the releasing rate of ibuprofen sustained-release capsules by near infrared transmission spectroscopy technology and chemometrics. Methods: A total of 30 batches of ibuprofen sustained-release capsules were chosen for analysis.First,the near infrared spectrum of the releasing liquid of ibuprofen sustained-release capsules was collected in different periods.Then,the active pharmaceutical ingredient(API) contents were determined by HPLC.Finally,the releasing rate quantitative model with the partial least square(PLS) algorithm available in the Quant 2 was developed. Results: Our model was based on 101 data obtained from 30 batches of samples,which included 61 data in calibration set with the API ranged from 4.97%-30.89%,and 40 data in test set with the API from 5.07%-30.34% .The spectra ranges were 8937-7487 cm^-1and 6102-5446 cm^-1;the pretreatment method was first derivation and multiple scatter correction;the rank was 6.In the cross validation,the values of R² and RMSECV were 95.04% and 1.96%(mg·mg^-1),respectively.In the external validation,the values of R² and RMSEP were 94.37% and 2.04%(mg·mg^-1),respectively. Conclusion: The method was accurate,quick and convenient,which could be used for quick analysis in drug control.

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