顶空固相微萃取气质联用法分析水中两种内分泌干扰物

Determination of Two Endocrine Disrupting Chemicals in Environmental Water Samples by Headspace Solid-Phasemicroextraction Coupled with Gas Chromatography-Massspectrometry(GC-MS)

建立了一种采用65μm聚二甲基硅氧烷/二乙烯基苯(PDMS/DVB)萃取头,顶空固相微萃取与气相色谱质谱联用快速分析水中对特辛基苯酚和4-正壬基酚两种内分泌干扰物的方法。采用PDMS/DVB(65μm)纤维头,于80℃下萃取30 min,萃取过程中以250 r/min的速度进行搅拌,萃取结束后,270℃下解吸6 min,对萃取纤维、萃取温度、萃取时间和解析时间等参数进行了优化。结果表明:在该优化参数下对特辛基苯酚和4-正壬基酚均在0.05~1.0μg/L范围内呈良好线性关系,相关系数R^(2)均大于0.995,对特辛基苯酚和4-正壬基酚方法检出限分别为0.03和0.01μg/L,并分别进行了低、中、高三种水平浓度的6次平行加标回收率测试,加标回收率为85.4%~103.1%,相对标准偏差为3.2%~5.4%。该方法中内分泌干扰物无需衍生,简便快速,检出限低,重现性好,可用于水质中这两种内分泌干扰物的快速检测分析。

A new rapid and simple method based on headspace solid-phase microextraction(HS/SPME)coupled with gas chromatography-mass spectrometry was developed for the determination of 4-n-nonylphenol(4-n-NP)and 4-tert-Octylphenol(4-t-OP)in water with the Polydimethylsiloxane/Divinylbenzene(PDMS/DVB)fiber(65μm).Parameters of the extraction conditions were optimized,such as SPME fiber,extraction time,extraction temperature and adsorption time.The results showed that better recoveries were obtained with the PDMS/DVB fiber(65μm).The extraction was processed under 80℃and lasted for 30 min.The stirring speed was 250 r/min.The adsorption temperature was 270℃and lasted for 6 min.The method showed a good linear relationship for 4-n-NP and 4-t-OP in the range of 0.05~1.0μg/L,the correlation coefficient(R^(2))higher than 0.995,and the detection limit of 4-n-NP and 4-t-OP were 0.03 and 0.01μg/L.the recovery rates was in the range of 85.4%~103.1%with low,medium and high concentrations and the relative standard deviations(RSD)was in the range of 3.2%~5.4%(n=6).The method is simple,rapid,accurate,sensitive and repeatable,and can meet the requirements for the detection of 4-n-NP and 4-t-OP in water.