本文应用固相萃取前处理方法和高效液相色谱-三重四极杆电喷雾质谱(HPLC-ESI/tqMS),优化并建立了9种氯代和溴代乙酰胺的同时测定方法.结果显示,在流动相甲醇/水(5/95,V/V)、流速0.3 mL· min-1、正离子模式条件下,9种卤乙酰胺的线性范围是5-200 μg·L-1或10-500μg·L-1(R2 ＞0.99),9种卤乙酰胺检出限为0.5-9.2 μg·L-1.经过比较HLB是最优的固相萃取柱.在0.02、0.2、0.5 μg·L-1的3个加标水平下,9种卤乙酰胺的回收率分别为61％-84％、60％-93％和70％-104％,相对标准偏差为1.7％-4.4％、1.1％-4.1％和0.8％-4.1％.
In this study,a new method for the simultaneous determination of nine chlorinated and brominated haloacetamides in drinking water was developed using solid phase extraction (SPE) and high performance liquid chromatography-triple quadropole mass spectrometry (HPLC-tqMS) with positive electron spray ionization.The optimized HPLC mobile phase was composed of methanol and water (5/95,V/V) with a flow rate of 0.3 mL· min-1.The linear ranges of the HPLC-tqMS method were 5-200 μg· L-1 or 10-500 μg·L-1 (R2＞0.99) for the nine haloacetamides.The detection limits of the nine haloacetamides were 0.5-9.2 μg· L-1.HLB column was found to be the optimal SPE column.With the spiked concentrations of 0.02,0.2 and 0.5 μg·L-1,the recovery rates of the nine haloacetamides were 61％-84％,60％-93％ and 70％-104％,respectively (relative standard deviations were 1.7％-4.4％,1.1％-4.1％ and 0.8％-4.1％,respectively).
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