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研究了一种可同时测定合成样品中溴酚磷及其杂质(四溴联苯二酚和环磷酸酯)含量的高效液相色谱法.用MicropakMGH色谱柱,柱温40℃,流动相为乙腈-甲醇-水-醋酸(26∶57∶17∶0.2,v/v),紫外检测波长298nm,在本色谱条件下,各组份得到较好地分离.在实验的范围内线性关系良好,cv%≤2%,溴酚磷、四溴联苯二酚和环磷酸酯的检出限分别为24、10和14ng.本法优于紫外分光光度法(用于溴酚磷测定)和薄层层析法(用于杂质测定).
A high performance liquid chromatography (HPLC) method was developed for the simultaneous determination of bromopheno-P and its impurities (tetrabromophenol and cyclic phosphates) in synthetic samples. Using MicropakMGH column, the mobile phase was acetonitrile-methanol-water-acetic acid (26:57:17:0.2, v / v) with a UV detection wavelength of 298 nm at a column temperature of 40 ℃. Under the chromatographic conditions, Get better separation. The linear relationship was good in the experimental range. The detection limits of bromophenophene, tetrabromophenol and cyclophosphate were 24, 10 and 14 ng, respectively, for cv% ≤2%. This method is superior to UV spectrophotometry (for determination of bromophenolphosphate) and thin-layer chromatography (for impurity determination).