高效液相色谱法测定面粉及面粉制品中乙二胺四乙酸二钠的含量

在未使用离子对试剂和高盐缓冲液条件下,采用亲水性C_(18)反相液相色谱柱,以甲醇-水体系为流动相,建立了面粉及面粉制品中乙二胺四乙酸二钠含量的高效液相色谱测定方法。样品采用水溶液提取,在超声辅助下与三氯化铁反应生成稳定的衍生产物,用三氯甲烷净化衍生产物。采用高效液相色谱法以pH 4.0甲醇-水溶液(10∶90,体积比)为流动相,亲水性C_(18)反相液相色谱柱为固定相,260 nm波长下测定面粉及面粉制品中乙二胺四乙酸二钠含量。乙二胺四乙酸二钠的质量浓度在1.0~50.0 mg/L范围内呈良好的线性关系,其相关系数为0.999 6,检出限为3.0 mg/kg,定量下限为10.0 mg/kg。面粉样品添加浓度在10.0~200 mg/kg范围内,加标回收率为95.0%~103%,相对标准偏差为4.0%~6.3%,可满足面粉及面制品中乙二胺四乙酸二钠的快速检测和定量分析要求。

Determination of Disodium Ethylenediaminotetraacetic Acid in Flour and Its Products by High Performance Liquid Chromatography

In the absence of ion-pair reagents or high-salt buffer condition,a novel method for the quantitative analysis of disodium ethylenediaminotetraacetic acid in flour and its products by high performance liquid chromatography was developed,employing hydrophilic C18 reversed-phase liquid chromatography column and methanol-water system as mobile phase.Samples were extracted with aqueous solution,and reacted with ferric chloride by ultrasound irradiation to product stable derivative which was cleaned up with trichloromethane.To determine ethylenediaminotetraacetic acid disodium in flour and flour products,the analytes were determined by high performance liquid chromatography with a wavelength of 260 nm and a hydrophilic C18 reversed phase liquid chromatography column using mobile phases of pH 4.0 methanol and aqueous solution(10 ∶ 90,by volume).Under the optimal conditions,the calibration curves of the analytes were linear in the concentration range of 1.0-50.0 mg/L with the correlation coefficients of 0.999 6.The limits of quantification(LOQs) were 10.0 mg/kg,and the limits of detection(LODs) were 3.0 mg/kg.At spiked levels of 10.0-200 mg/kg,the average recoveries of spiked samples ranged from 95.0％ to 103％,with relative standard deviations between 4.0％ and 6.3％.The method could meet the requirement for the rapid screening and quantitative analysis of disodium ethylenediaminotetraacetic acid in flour and its products.