水中16种邻苯二甲酸酯类稳定性同位素内标-自动固相萃取-气质联用测定

Determination of 16 phthalate esters in water by automatic solid-phase extraction and gas chromatography-mass spectrometer coupled with stable isotope internal standard

目的建立稳定性同位素内标-自动固相萃取-气质联用测定水中16种邻苯二甲酸酯类(PAEs)的方法,并应用于水质分析。方法 2016年1—2月采集福建省福州某医院血液透析科、闽江、居民家中和某大型超市水样各1 L,气相色谱-质谱联用(GC-MS)分析,内标法定量。测定透析水,江水、管网末梢水、地下水等实际水样,并以实际水样为本底,进行低、中、高3种浓度水平的加标实验(n=6),计算回收率与相对标准偏差(RSD)。结果 4类水体均含有邻苯二甲酸二异丁酯(DIBP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2–乙基)己酯(DEHP)等PAEs,浓度0.041~0.843μg/L,方法检出限(MDL)为0.005~0.017μg/L,方法定量限(LOQ)0.015~0.051μg/L,回收率为74.0%~118%,RSD为1.1%~20%。结论该方法克服了手动固相萃取缺点,水样处理效率高,准确,可靠,适用于水中PAEs的检测。

Objective To establish a gas chromatography-mass spectrometer （GC-MS） method with solid-phase extraction and stable isotope internal standard for the detection of 16 phthalate esters （PAEs） in water samples.Methods Four kinds of one liter water sample （hemodialysis water, ground water, tape water, and bottled underground water） were collected in a hospital, Min River, a residential house, and a super market in Fuzhou city of Fujian province; between January and Feburary 2016, and then the PAEs in the sample were detected with GC-MS. The samples were quantified with internal standard method and the samples were also spiked at low, medium and high levels to evaluate recovery rate and relative standard deviation （RSD） of the assays.Results PAEs, including diisobutyl phthalate （DIBP）, dibutyl phthalate （DBP）, and （2-ethylhexyl） phthalate （DEHP）,were detected in the 4 kinds of water samples with the concentrations ranging from 0.041 μg/L-0.843 μg/L. The method detection limits were 0.005 μg/L-0.017 μg/L and the limits of quantitation were 0.015 μg/L-0.051 μg/L. The recoveries of 3 spiked concentrations in 4 kinds of water were 74.0%-118.4% and the RSD was 1.1%-20.0%.Conclusion The method overcomes shortcoming of manual solid-phase extraction, and is of high efficiency, good accuracy, stability and practicability, could be used in detection of PAEs in water samples.