近红外光谱法快速分析注射用头孢曲松钠及其水分的含量

Development of a near-infrared method for rapid determination of ceftriaxone and water content in ceftriaxone sodium for injection

目的:利用近红外漫反射光谱(NIRDRS)分析技术和化学计量学方法对注射用头孢曲松钠及其水分进行无损、快速定量分析。方法:以全国不同企业生产的注射用头孢曲松钠为分析对象,用光纤测定近红外漫反射光谱,采用偏最小二乘法(PLS)算法建立模型。结果:注射用头孢曲松钠定量分析模型由60个样品经内部交叉验证建立,85个样品用于外部验证,浓度范围为72.1%～90.6%,相关系数为0.9712,交叉验证均方差(RMSECV)为1.21.外部验证均方差(RMSEP)为1.07。注射用头孢曲松钠水分定量分析摸型由56个样品经内部交叉验证建立,62张光谱用于外部验证,浓度范围为2.8%～9.9%,相关系数为0.9930,RMSECV 为0.271,RMSEP 为0.294。结论:2个模型结合可以按药典要求对注射用头孢曲松钠含量进行快速预测,方法怏速、简便,可用于药品的现场快速分析。

Objective： A near - infrared （NIR） quantitative method was developed for rapid and nondestructive determination of ceftriaxone and water content in ceftriaxone sodium for injection. Methods：The diffuse reflectance nearinfrared spectra of ceftriaxone sodium for injection from different pharmaceutical factories in China were measured intactly by a fiber optic probe. The calibration model was developed using partial least squares （PLS） algorithm. Result： For the quantitative model of ceftriaxone content, 60 batches of ceftriaxone sodium for injection samples were used as calibration set, and 85 batches as validation set. The concentration range was 72. 1% - 90. 6% , and the correlation coefficient of cross validation was 0. 9712, the root mean square error of cross validation （RMSECV） was 1.21% and the root mean square error of prediction （RMSEP） was 1.07%. For the quantitative model of water content,56 batches of ceftriaxone sodium for injection samples were used as calibration set, and 62 batches as validation set. The concentration range was 2. 8% -9.9%, and the correlation coefficient of cross validation was 0. 9930, the RMSECV was 0. 271% and the RMSEP was 0. 294%. Conclusion：Using the two quantitative models,we can quickly evaluate the ceftriaxone sodium for injections according to ChP. The method is simple and rapid, the NIRDRS result can be used in the mobile lab.