摘要
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 develop a model for rapid and non-destructive determination of amoxilcillin sodium and sulbactam sodi- um for injection using the analysis of near infrared diffuse reflectance spectroscopy （NIR） and chemometrics. Methods： Totally 41 batches of commercial samples and 20 batches of laboratory samples were analyzed by NIR and the legal methods. The first derivative and vector normalization were selected as the preprocessing methods and 8 720-5 446 cm-1 was selected as the frequency range. Results： The quantitative model was constructed based on 16 batches of commercial samples and 15 batches of laboratory samples （0.75 g） and the content ranged from 4.45% to 61.82% for amoxilcillin and 15.75% to 30.25% for sulbactam. The root mean square errors of cross validation （RMSECV）, determination coefficients （g2） and root mean square errors of prediction （RMSEP） respectively was 0. 858, 0. 998 1 and 0.936 for amoxileillin, and respectively was 0. 541, 0. 988 1 and 0.423 for sulbactam. The model was tested based on 5 batches of commercial samples and 5 batches of laboratory samples （0.75 g） and the results well met with those of the legal methods with difference ≤ 1.5%. The model also applied in 10 batches of commercial samples （ 1.5 g） and 2 batches of samples from the other manufacturers. Conclusion： The non-destructive quantitative NIR methods are accurate with good reproducibility, and appli- cable for the rapid analysis of amoxilcillin sodium and sulbactam sodium for injection.
出处
《中国药师》
CAS
2017年第8期1496-1498,共3页
China Pharmacist
关键词
近红外漫反射光谱
注射用阿莫西林钠/舒巴坦钠
定量模型
Near infrared diffuse reflectance spectroscopy
Amoxilcillin sodium and sulbactam sodium for injection
Quantitative model
