高效液相色谱法测定合成样品中溴酚磷及其杂质含量的研究

Study of HPLC Method for Determination of Bromophenophos and It's Impures

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 HPLC method has been developed for the simultaneous determination of Bromophenophos (Ⅰ) and it's impures [Tetrabromodiphenyldiol (Ⅱ) and tetrabromodiphenyldiol cyclic phosphate (Ⅲ)]. The column used was a Micropak MCH column. The mobile phase was a mixture of acetonitril methol water acetic acid (26∶57∶17∶0.2, v/v). The wavelength of UV detection was 298 nm and the temperature of column was 40℃. Under the chromatographic conditions, the components can be separated well. The linear relationship was good for the concentration range under investigation and the variation coefficient was less than 2%. The detection limits of (Ⅰ), (Ⅱ) and (Ⅲ) were 24ng, 10ng and 14ng, respectively. This HPLC method is better than UV method (for the determination of Ⅰ) and TLC method (for the determination of Ⅱ,Ⅲ).