重氮-偶联反应间接光度法测定药物中美司钠  

Indirect photometric method for determination of sodium 2-sulfanylethanesulfonate in pharmaceuticals with diazo-coupling reaction

作　　者：李倩[1] 马卫兴[1,2] 

机构地区：[1]淮海工学院化学工程学院,连云港222005 [2]淮海工学院药学院,连云港222005

出　　处：《分析试验室》2017年第5期589-592,共4页Chinese Journal of Analysis Laboratory

摘　　要：基于在H_2SO_4介质中,利用IO_3^-氧化美司钠后剩余的IO_3^-紧接着氧化盐酸羟胺产生NO_2^-,新生的NO_2^-使对氨基苯磺酸发生重氮化反应,生成对氨基苯磺酸重氮盐,该重氮盐再与盐酸萘乙二胺反应生成紫红色的偶氮染料,提出了利用重氮化-偶联反应间接分光光度测定美司钠含量的方法。方法中反应产物是一种有机偶氮染料,其最大吸收波长在522 nm处,工作曲线的线性范围在1.0~12 mg/L,摩尔吸光系数为1.296×10~5L·mol^(-1)·cm^(-1)。考察了各试剂用量对产物的影响,找出了该方法的最佳反应条件。用所建立的重氮化-偶联反应间接光度法测定了注射剂中美司钠的含量,方法的回收率在99.3%~101.2%之间,样品测定的相对标准偏差为0.82%和0.54%。A new sensitive and simple method by using indirect spectrophotometry for the determination of mesna in pharmaceuticals was proposed firstly. The procedure is based on diazo-coupling reaction of N-（ 1-naphthyl） ethylenediamine dihydrochloride and diazonium salt of sulfanilic acid. Mesna is first oxidized by excess potassium iodate in dilute sulfuric acid medium,and the excessive amounts of potassium iodate next oxidizes hydroxylamine hydrochloride to form nitrite ion. Then diazo reaction occurs between the new born nitrite ion and sulfanilic acid to produce the diazonium salt of sulfanilic acid,which is finally coupled with N-（ 1-naphthyl） ethylenediamine dihydrochloride,yielding an organic amaranthine azo dye for spectrophotometric measurements. Beer＇s law was obeyed in the range1. 0 ～ 12 mg/L of mesna with maximum absorption wavelength at 522 nm. Its molar absorption coefficient was 1. 296 × 10^5 L · mol^-1·cm^-1. The effect of the reagent dosage on the product was investigated and the optimal analytical conditions were evaluated. The proposed indirect spectrophotometric method based on diazo-coupling reaction was applied to determine the content of sodium 2-sulfanylethanesulfonate in mesna injection, and satisfactory results are obtained. The recoveries between 99. 2% ～ 103. 0% and the relative standard deviations of determination for sample are 0. 82% and 0. 54%.

关 键 词：美司钠 重氮化-偶联反应 间接光度法 

分 类 号：R917[医药卫生—药物分析学]