摘要
目的建立在线监测注射用头孢唑林钠干燥过程中的水分含量测定方法。方法水分定量模型建模样品采以不同批次、不同干燥时间段五水头孢唑林钠原料为研究对象,结合干燥、引湿实验扩充样品水分范围,用积分球测定近红外漫反射光谱,并采用聚类分析挑选出建模光谱,光谱预处理方法为一阶导数+MSC法,谱段为7502~6499.2、5500.2~3 999.8 cm^(-1),回归方法偏最小二乘法。结果水分定量模型建模样品共计85个,水分含量质量分数为12.15%~16.41%,相关系数(coefficient of determination,R^2)为96.30,交叉验证均方差(root mean square error of cross validation,RMSECV)为0.181。外部验证样品52个,水分含量质量分数为13.28%~16.17%,外部验证均方差(root mean square error of predication,RMSEP)为0.149。模型专属性强,准确度、线性和精密度符合要求。结论建立的运用近红外监测注射用头孢唑林钠干燥过程的水分含量方法是可行的,为实现近红外在线干燥提供了实验基础。
Objective To construct a quantitative model for on-line drying process endpoint detection of water in cefazolin sodium pentahydrate powder for injection using near infrared（ NIR） spectroscopy technology.Methods Multiple bathes of cefazolin sodium pentahydrate powder from different time points of drying process were collected and used for cluster analysis combined with vacuum dry experiments and wet experiments to construct the water quantitative model. The first derivative followed by MSC method was used for spectra pretreating and 7 502 ~ 6 499. 2 cm^（-1） and 5 500. 2 ~ 3 999. 8 cm^（-1） were selected as the frequency range. The calibration model was developed using the partial least squares（ PLS）. Results This quantitative model was constructed with 85 samples. The water content of cefazolin sodium ranges from12. 15% to 16. 41%. The correlation coefficient of the calibration curve（ R^2） was 96. 30. The root mean square error of prediction（ RMSECV） of model was 0. 181. 52 samples were used as validation set, the water content of cefazolin sodium ranges from 13. 28% to 16. 17%,and the root mean square error of prediction（ RMSEP） was 0. 149. In addition, the quantitative model was evaluated in terms of specificity, linearity,accuracy,and precision. Conclusions Conclusions It is feasible to construct a universal quantitative model for the measurement of water content in of cefazolin sodium pentahydrate powder. The quantitative model could be applied in the quick assay of the water content of cefazolin sodium pentahydrate powder produced（ content： 12. 15%-16. 41%）. It provides an experimental basis to achieve a NIR method used in routine drying process.
作者
易夏
冯艳春
胡昌勤
赵春杰
YI Xia FENG Yan-chun HU Chang-qin ZHAO Chun-jie(School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China Shenzhen China Resources Gosun Pharmaceutical Group, Shenzhen 518049, China National Institutes for Food and Drug Control ,Beijing 100050, China)
出处
《沈阳药科大学学报》
CSCD
北大核心
2017年第7期558-564,574,共8页
Journal of Shenyang Pharmaceutical University
基金
深圳市战略新兴产业发展专项资金资助项目(编号CXZZ20130508105318972)
关键词
近红外光谱法
过程分析技术
头孢唑林钠
水分
定量模型
干燥过程
near-infrared spectra
process analytical technology
cefazolin sodium pentahydrate
water
quantitative analysis
drying process
