超声萃取-气相色谱-质谱法测定空气颗粒物中邻苯二甲酸酯类化合物

Determination of phthalatic-acid esters in air particulates by ultrasonic extraction-gas chromatography-mass spectrometry

目的建立空气颗粒物PM10和PM2.5中邻苯二甲酸酯类化合物的超声萃取-气相色谱-质谱检测方法。方法运用内标法,使用正己烷作为溶剂,经超声萃取法提取滤膜中16种邻苯二甲酸酯后用气相色谱-质谱法测定。结果 16种邻苯二甲酸酯类化合物均能准确定量,在0.5 mg/L^10.0 mg/L范围内相关系数>0.999,最低检出限为0.000 6 mg/L^0.039 5 mg/L,回收率为75.21%~128.91%。所检居民住宅室内空气颗粒物样本中DIBP、DBP、DCHP、DEHP 4种化合物均有检出,其他组分未检出。结论本方法操作简单,测定成本低,准确度和精密度良好,可应用于空气颗粒物中邻苯二甲酸酯类化合物的定量分析。

Objective A method was developed for the determination of phthalatic-acid esters in PM10 and PM2.5 by ultrasonic extraction and gas chromatography-mass spectrometry.Methods Sixteen phthalates in quartz filters were extracted by ultrasonic extraction with n-hexane and determined by gas chromatography coupled mass spectrometry using internal standard.Results All 16 phthalate esters could be quantified accurately.The correlation coefficients were over 0.999 in the range of 0.5 mg/L to 10.0 mg/L.The detection limits ranged from 0.0006 mg/L to 0.0395 mg/L.The recovery rates were within 75.21%-128.91%.Four compounds,DIBP,DBP,DCHP and DEHP,were detected in indoor air particulate matters samples from residences,while other analogues were not found.Conclusion The method was simple,accurate and reliable,and it is suitable for quantitative analysis of phthalate esters in air particulates.