柱前衍生-EI源串联四极杆气质联用测定地表水中的丙烯酰胺

Determination of Acrylamide in Surface Water by GC-EI-MS/MS

建立了地表水中痕量丙烯酰胺的柱前衍生-EI源串联四极杆气质联用测定方法。丙烯酰胺的双键经溴化衍生成2,3-二溴丙酰胺,加入硫酸钠盐析,乙酸乙酯萃取,浓缩取1μl进样,由串联四极杆气相色谱质谱联用仪测定。通过MRM（150→70.0/107.0）多反应监测实现定性和外标法定量分析。与其他方法相比,该方法具有定性准确、灵敏度高的特点。方法检出限为0.03μg/L,线性范围在0.030-40μg/L;相关系数r=0.9998;六次测定值RSD在14.3%;回收率在89%-196%之间,结果满意。

It was established a method to. determine trace amounts of acrylamide monomer in aqueous matrices especially surface water by GC with tandem MS. This method is based on bromination of the acrylamide double bond. The reaction product （2,3-dibromopropionamide） is extracted from the reaction mixture with ethyl acetate, after salting out with sodium sulfate. The extract is analyzed by gas chromatography with tandem MS detection （GC-MS/MS）. The method detection limit （MDL） in an aqueous matrix is 0.030μg/L, linear range is 0.030 - 40μg/L,relative coefficient is 0.9998, RSD = 14.3% （n = 6） and recovery is 89% - 196% .