溴乙酰溴中二溴乙酰溴杂质分析方法的研究

Determination of Dibromoacetyl Bromide Impurity in Bromoacetyl Bromide

建立了间接测定溴乙酰溴中二溴乙酰溴含量的HPLC方法。将溴乙酰溴水解生成溴乙酸,辅以LC-MS技术,对其主要杂质进行定性研究。采用十八烷基硅烷键合硅胶柱,流动相为V(10 mmol/L三乙胺溶液)∶V(乙腈)=95∶5,检测波长为205 nm。溴乙酸与二溴乙酸在0.001~1.0 mg/mL浓度范围内线性关系良好,平均回收率为99.3%,RSD为0.87%,二溴乙酸相对校正因子为0.37。高效液相色谱法与离子色谱法测定结果一致,方法准确可靠,适于对溴乙酰溴原料中二溴乙酰溴杂质的控制。

HPLC method was established for indirectly determining dibromoacetyl bromide impurity in bromoacetyl bromide.Bromoacetyl bromide was hydrolyzed into bromoacetic acid and a LC-MS method was used to do qualitative analysis of the main impurities in bromoacetyl bromide.A Thermo Acclaim 120 C18 column was used with the mobile phase of 10 mmol/L triethylamine solution（adjusted to pH 5.0 with phosphoric acid）∶acetonitrile（95∶5） at the detection wavelength of 205 nm.It was linear in the concentration range of 0.001-1.0 mg/mL for bromoacetic acid and dibromoacetic acid.The average recovery of dibromoacetic acid was 99.3%,with RSD of 0.87%.The relative correcting factors of dibromoacetic acid was 0.37.The quantitative result was no significant difference between using HPLC and ion chromatography.This method is accurate and reliable,and is suitable for detection of dibromoacetyl bromide in bromoacetyl bromide.