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建立了乙二胺四乙酸盐(EDTA)和二乙烯三胺五乙酸盐(DTPA)衍生化成乙基酯的前处理方法以及气相色谱-质谱法测定乙基酯的方法。样品经甲酸酸化后,与乙醇发生酯化反应生成乙基酯,由正己烷提取,选择离子模式下由优化好的气相色谱-质谱进行定性定量分析。EDTA和DTPA质量浓度分别在0.2~20.0 mg/L和0.5~50.0 mg/L范围内线性关系良好,相关系数均不小于0.9991,两种不同阴性样品的3个不同浓度添加水平的平均回收率在91.6%~94.9%之间,相对标准偏差均不大于5.2%,EDTA和DTPA检出限分别为0.0609 mg/kg和0.145 mg/kg,定量限分别为0.194 mg/kg和0.476 mg/kg。方法能够满足染整助剂中EDT A和DT PA定性确证和准确定量的要求。
The pretreatment methods of derivatization of ethylenediaminetetraacetate (EDTA) and diethylenetriaminepentacetate (DTPA) to ethyl esters and the determination of ethyl esters by gas chromatography-mass spectrometry were established. After the sample was acidified with formic acid, it was esterified with ethanol to form ethyl ester. The product was extracted with n-hexane and qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry with optimized ion mode. The linear relationship between EDTA and DTPA concentrations was 0.2 ~ 20.0 mg / L and 0.5 ~ 50.0 mg / L, respectively. The correlation coefficient was not less than 0.9991. The average recovery of three different concentrations of EDTA and DTPA was The relative standard deviations were no more than 5.2%. The detection limits of EDTA and DTPA were 0.0609 mg / kg and 0.145 mg / kg, respectively. The limits of quantification were 0.194 mg / kg and 0.476 mg / kg, respectively. The method can meet the requirement of qualitative confirmation and accurate quantification of EDT A and DT PA in dyeing and finishing auxiliaries.