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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 establish a method for the determination of 15 kinds of phthalates (PAEs) in water by gas-assisted liquid-liquid microextraction (AALLME) -chromatographic-triple quadrupole mass spectrometry (GC-MS) Methods Gas chromatography-assisted liquid / liquid microextraction (AALLME) was used to enrich the samples and centrifuge them. EI sources were used for quantification by external standard method under selective ion scan (SIM) mode. Results When the concentration of 15 phthalates was between 100.0 ng / L and 1 000 ng / L, the correlation coefficient (r) was 0.994 9 to 0.999 9, and the detection limit was 10.9 ng / L ~ 37.4 ng / L, the limit of quantification was 38.9 ng / L ~ 100.0 ng / L, the spiked recoveries were 75.9% ~ 124.6% and the relative standard deviations were 7.6% ~ 16.5%. The enrichment multiple of the method is 759 times to 1 246 times. Conclusion The method is simple, rapid and reliable, eliminating the use of dispersants, increasing the enrichment factor, reducing the interference of complex matrix and increasing the sensitivity of the target compounds. It can be used in 15 kinds of o-phthalic acid Determination of formate.