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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%。
Based on the use of IO_3 ~ - in the H_2SO_4 medium, the remaining IO_3 ~ - after the oxidation of mesna sodium followed by the oxidation of hydroxylamine hydrochloride to produce NO_2 ~ -, the new NO_2 ~ - sulfanilic acid diazotization reaction to generate amino Benzenesulfonate diazonium salt, the diazonium salt reacts with naphthyl ethylenediamine hydrochloride to form a fuchsine azo dye, and a method of indirect spectrophotometric determination of mesna using diazotization-coupling reaction is proposed. The reaction product is an organic azo dye with a maximum absorption wavelength at 522 nm. The linear range of the working curve is 1.0-12 mg / L and the molar absorption coefficient is 1.296 × 10 -5 L · mol -1. · Cm ~ (-1). The effect of the amount of each reagent on the product was investigated, and the optimum reaction conditions for the method were found out. The diazotization - coupling reaction indirect spectrophotometry was used to determine the content of mesna in the injection. The recoveries were between 99.3% and 101.2%, and the relative standard deviations (RSDs) were 0.82% and 0.54%, respectively.