拉曼光谱法研究呋塞米晶型及其定量模型的建立  

Analysis of the Polymorphism of Furosemide by Raman Spectroscopy and Establishment of the Quantitative Model

作　　者：黄蓉 叶晓霞[1] 陆丹[1] 毛丹卓[1] 杨永健[1] HUANG Rong;YE Xiao-xia;LU Dan;MAO Dan-zhuo;YANG Yong-jian(Shanghai Institute for Food and Drug Control,Shanghai 201203,China)

机构地区：[1]上海市食品药品检验所,上海201203

出　　处：《中国药学杂志》2018年第24期2127-2131,共5页Chinese Pharmaceutical Journal

基　　金：国家重大科学仪器设备开发专项资助(2012YQ180132);药典会药品医疗器械审评审批制度改革专项课题资助(ZG2017-4-02)

摘　　要：目的采用拉曼光谱法研究呋塞米晶型及其定量模型的建立。方法建立呋塞米3种晶型的拉曼对照图谱,用TQ Analyst数据分析系统建立呋塞米晶型定量模型。结果应用偏最小二乘法(PLS)建立回归模型,采用多元信号修正(MSC),标准正则变换(SNV)和1~2阶导数等不同的数据预处理算法来减少系统干扰。所建立的定量模型对于晶型Ⅰ,Ⅱ,Ⅲ的均方差(RMSEC)分别为0. 098 6,0. 366,0. 051 7,相关系数r分别为1. 000 0,0. 999 9,1. 000 0。验证集样品预测值与其实际值之间的预测均方差(RMSEP)分别为0. 065,0. 070 4,0. 012,因子factors分别为8,8,9。结论拉曼光谱测定方法和该定量模型可用于呋塞米晶型判别及定量。OBJECTIVE To analyze the polymorphism of furosemide by Raman spectroscopy and establish the quantitative model. METHODS The reference Raman spectra of the three crystal forms of furosemide were established,and a quantitative model wasestablished by TQ Analyst data analysis system. RESULTS Partial least-squared( PLS) regression models were developed,and different data preprocessing algorithms such asmultiplicative signal correction( MSC),standard normal variate( SNV) and the 1 st to 2 nd derivatives were applied to reduce the influence of systematic disturbances. The root mean square errors of calibration( RMSEC) of the quantitative model established for form Ⅰ,Ⅱ,and Ⅲ were 0. 098 6,0. 366 0,0. 051 7,and the correlation coefficients( r) were1. 000 0,0. 999 9,and 1. 000 0,respectively; the root mean square errors of prediction( RMSEP) between the predicted value of the sample and its actual value were 0. 059 0,0. 070 4,0. 045 1,and the factors were 8,8,and 9,respectively. CONCLUSION Raman spectroscopy can be used to analyze the polymorphism of furosemide and the quantitative model can be used for quantitative determination of furosemide crystal form.

关 键 词：呋塞米 晶型 拉曼光谱法 定量 

分 类 号：R917[医药卫生—药物分析学]