气质联用测定生活饮用水中痕量邻苯二甲酸酯类物质的正交分析

Determination of trace amounts of phthalate esters in drinking water orthogonal analysis of material by Gas Chromatography/Mass Spectrometry

目的建立一种测定生活饮用水中邻苯二甲酸酯类有机污染物的固相萃取-气质联用的定性定量分析方法。方法采用固相萃取预处理和气质联用对10种邻苯二甲酸酯类物质(PAEs)进行测定,针对影响固相萃取的固相萃取柱、洗脱剂、洗脱时间3个主要因素,利用正交试验进行萃取条件的优化。结果最佳萃取条件:固相萃取柱为HLB固相萃取小柱(HLB柱),洗脱剂为乙酸乙酯,洗脱时间为25min,并确定了10种PAEs的相关系数≥0.98、最低检出限为0.03μg/L,回收率为87.3%～96.6%。结论正交试验得出的最佳萃取条件的检测方法线性相关性较好,精度高,准确性好,适于生活饮用水中痕量PAEs的测定。

Objective A gas chromatography method coupled with solid phase extraction（SPE） for the determination of trace phthalate esters（PAEs） in living and drinking water samples was developed.Methods The solid-phase extraction（SPE） Pre-treatment and GC-MS were used to determine ten phthalate esters（PEAs） in water.The orthogonal test of the three main factors influencing SPE was carried out.These include the SPE cartridge,type of eluting solvent and eluting time.Results The optimized extraction conditions of using HLB cartridge as SPE cartridge,Ethyl acetate as eluting solvent,25 min as eluting time,and the linear relativity was above 0.98,minimum detection limits was 0.03 μg/L and the recovery of ten PEAs were 87.3%~96.6%.Conclusion This method has better linear relativity,high precision and good accuracy,It adapts to determine the trace PEAs concentration in water.