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目的:利用近红外漫反射光谱(NIR)分析技术和化学计量学的方法,无损、快速的对注射用阿莫西林钠/舒巴坦钠进行定量分析。方法:采集41批原始样品及20批破坏样品的近红外漫反射光谱,同时以法定方法分别测得阿莫西林、舒巴坦的含量,光谱预处理方法为一阶导数+矢量归一化,谱段范围为8 720~5 446 cm~(-1)。结果:以0.75 g规格的16批原始样品及15批破坏样品作为校正集经交叉验证建立定量模型,阿莫西林、舒巴坦的浓度范围分别为4.45%~61.82%、15.75%~30.25%,交叉验证均方根误差(RMSECV)分别为0.858、0.541,确定系数(R~2)分别为0.998 1、0.988 1;以0.75 g规格的5批原始样品及5批破坏样品作为验证集Ⅰ进行外部验证,预测均方根误差(RMSEP)为0.936、0.423;预测结果与法定方法参考结果对比,偏差均在1.5%之内;以1.5 g规格的10批原始样品及2批不同生产企业样品作为验证集Ⅱ,结果与法定结果一致,说明此模型通用于两种规格、适用性强。结论:此方法快速、可靠,可在安瓿瓶外无损采集光谱,可用于药品的快速定量分析。
OBJECTIVE: To quantitatively analyze amoxicillin / sulbactam sodium for injection nondestructively and rapidly using near-infrared diffuse reflectance spectroscopy (NIR) and chemometric methods. Methods: The near-infrared diffuse reflectance spectra of 41 batches of raw samples and 20 batches of damaged samples were collected. At the same time, the content of amoxicillin and sulbactam was measured by the statistic method. The first order derivative and vector normalization were used as the pretreatment method. The spectral range is 8 720 ~ 5 446 cm -1. Results: Quantitative models were established by cross validation of 16 batches of raw samples of 0.75 g and 15 samples of destructive samples. The concentrations of amoxicillin and sulbactam were 4.45% -61.82% and 15.75% -30.25%, respectively. The root mean square error of cross-validation (RMSECV) were 0.858,0.541, and the determination coefficients (R ~ 2) were 0.998 and 1,0.9881 respectively. Five batches of original samples of 0.75 g and five batches of samples were used as validation sets. The root mean square error of prediction (RMSEP) was 0.936 and 0.423 respectively. The predicted results were within 1.5% of the statutory reference values. The samples of 10 batches of 1.5 g standard samples and 2 batches of samples of different manufacturing enterprises were used as verification Set Ⅱ, the result is consistent with the statutory results, indicating that this model is common to both specifications and has strong applicability. Conclusion: This method is fast and reliable, and can be used for non-destructive collection of ampoules. It can be used for rapid quantitative analysis of drugs.