气体辅助液/液微萃取-气相色谱-三重四极杆质谱联用法测定生活饮用水中的15种邻苯二甲酸酯

Determination of 15 phthalate esters in drinking water by gas chromatography triple quadrupole mass spectrometry after air-assisted liquid-liquid microextraction

目的建立气体辅助液/液微萃取(AALLME)-气相色谱-三重四极杆质谱(GC-MS)测定水中15种邻苯二甲酸酯(PAEs)的方法。方法采用气体辅助液/液微萃取技术(AALLME)富集,离心分离,使用EI源,选择离子扫描(SIM)模式下外标法定量检测。结果 15种邻苯二甲酸酯的浓度为100.0 ng/L^1 000 ng/L时,线性关系良好,相关系数(r)为0.994 9~0.999 9,方法的检出限为10.9 ng/L^37.4 ng/L,定量限为38.9 ng/L^100.0 ng/L,加标回收率为75.9%~124.6%,相对标准偏差为7.6%~16.5%。方法的富集倍数为759倍~1 246倍。结论本方法简单、快速、可靠,免去了分散剂的使用,提高了富集倍数,减少了复杂基质的干扰,提高了目标化合物的灵敏度,可以用于生活饮用水中的15种邻苯二甲酸酯的测定。

Objective To develop a method for the determination of 15 phthalate esters in drinking water by gas chromatography triple quadrupole mass spectrometry after air-assisted liquid-liquid microextraction（AALLME）.Methods PAEs in water sample were extracted and enriched by air-assisted liquid-liquid microextration（AALLME） and then determined by GC-MS in the selected ion monitoring（SIM） mode.The quantification was based on external standard method.Results The method showed good linear relation when the concentration of the 15 phthalate esters were within 100.0 ng/L-1 000 ng/L.The correlation coefficient（r） was within 0.994 9-0.999 9.The limits of detection were within 10.9 ng/L-37.4 ng/L,and the limits of quantification were within 38.9 ng/L-100 ng/L.The average spiked recoveries of the method were within 75.9%-124.6%,with the relative standard derivations（RSDs） of 7.6%-16.5%.The enrichment factors were within 759-1 246.Conclusion The method is simple,rapid and reliable.The method uses no disperser solvent and increases enrichment factors.The interference of the complex matrix is reduced,and the sensitivity of the target compound is improved.It is a suitable to the routine analysis of PAEs in water samples.