近红外光谱法快速分析注射用盐酸头孢甲肟及其水分的含量

Rapid Determination of Cefmenoxime and Moisture in Cefmenoxime Hydrochloride for Injection by Near-infrared Spectroscopy

关键词:  盐酸头孢甲肟  水分  近红外漫反射光谱  定量分析

Key words:  cefmenoxime hydrochloride  moisture content  near-infrared diffuse reflectance spectroscopy  quantitative determination

摘要:

目的 建立近红外通用性模型，对注射用盐酸头孢甲肟及其水分进行无损、快速定量分析。方法 以不同企业生产的注射用盐酸头孢甲肟为分析对象，用光纤测定近红外漫反射光谱，并通过聚类分析方法确定校正集和预测集，考察不同预处理方法、谱段的影响，选择建立最佳的注射用盐酸头孢甲肟及其水分的定量模型。结果 注射用盐酸头孢甲肟定量分析模型由36个校正集样品建立校正模型，17个样品用于外部验证，验证集相关系数为96.33%，校正集均方差为1.19%，验证集均方差为1.66%。注射用盐酸头孢甲肟水分定量分析模型由34个样品校正集样品建立校正模型，19个样品用于外部验证，验证集相关系数为96.39%，校正集均方差为0.22%，验证集均方差为0.26%。结论 2个模型结合可以对注射用盐酸头孢甲肟含量和水分进行快速测定，方法简便，结果准确可靠，适合大量重复性样品的分析测定。

Abstract:

OBJECTIVE To develop a universal near-infrared reflectance model for rapid and nondestructive determination of cefmenoxime and moisture in cefmenoxime hydrochloride for injection. METHODS Using cluster analysis method, cefmenoxime hydrochloride for injection from different pharmaceutical companies were measured by a fiber optic probe and were divided into calibration and validation groups. Then, the quantitative models were established using partial least square through selection of different wavelength ranges, preprocessing methods. RESULTS For the quantitative model of cefmenoxime content, 36 batches of samples were used as calibration set, and 17 batches as validation set. The root mean square error of calibration was 1.19%, and the root mean square error of validation was 1.66%, and correlation coefficients was 96.33%. For the quantitative model of water content, 34 batches of samples were used as calibration set, and 19 batches as validation set. The root mean square error of calibration was 0.22%, and the root mean square error of validation was 0.26%, and correlation coefficients was 96.39%. CONCLUTION Using this two quantitative models, cefmenoxime hydrochloride for injection can be quickly evaluated. The method is simple and rapid, and can be used in the mobile lab.