柱前衍生高效液相色谱法测定面制品中溴酸盐的含量

Determination of bromate content in flour by pre column derivatization HPLC

针对目前离子色谱电导法检测面制品中溴酸盐的假阳性问题,建立柱前衍生高效液相色谱测定面制品中的溴酸盐的方法。面制品经超纯水提取、过滤、衍生,采用C18色谱柱,紫外检测器检测。结果表明,采用亚铁氰化钾-乙酸锌作为沉淀剂,待测液在45℃时衍生60 min,溴酸盐浓度在0.025~1 mg/L范围内与峰面积呈现良好线性关系,方法的加标回收率为87.90%~94.80%,检出限为0.3 mg/kg,定量限为1 mg/kg。与离子色谱法相比,该方法具有干扰少,灵敏度高,成本低等优点,可很好地满足面制品中溴酸盐的检测和质控要求。

Aiming at the problem of false positive detection of the bromate ion chromatography in flour products,a method for bromate by pre column derivatization HPLC determination of flour products was established. Flour products were treated by ultrapure water extraction,filtration and derivative,than analyzed by C18 chromatographic column and UV detector. The results showed that,the reaction at 45 ℃ of 60 min derivative with the potassium ferrocyanide-zinc acetate was used to the precipitant solution,had a good linearity in the range of 0.025-1 mg/L.The recoveries were between 87.90% -94.80%,detection limit was0.3 mg/kg and quantitative limit was 1 mg/kg.This method was less interference than ion chromatography,with high sensitivity,and low cost.It was a good match for the detection of bromate in flour products and quality control requirements.