自动固相微萃取-气相色谱-三重四极杆质谱法直接测定水体中的多环芳烃

Direct Tetermination of Polycyclic Aromatic Hydrocarbons in Water by Automated Solid-Phase Microextraction Coupled with Gas Chromatography-Triple Quadrupole Mass Spectrometry

建立了固相微萃取(SPME)与气相色谱-三重四极杆质谱法(GC-MS/MS)联用直接测定水体中16种多环芳烃的快速分析方法。通过实验,对固相微萃取纤维涂层的选择、萃取时间、萃取温度等萃取条件以及碰撞电压等参数进行了优化。实验结果表明,采用涂层厚度为100μm的聚二甲基硅氧烷(PDMS)萃取头,以350转/分钟(r/min)40℃下搅拌萃取40min,在GC进样口经280℃热解析6min后,以气相色谱-三重四极杆质谱的多反应监测(MRM)模式检测。在0.2~4.0μg/L的线性范围内,该方法对水中16种PAHs所得的回归方程均具有较好的线性关系,相关系数r值为0.9953~0.9995,检出限为0.001~0.02μg/L。16种PAHs的0.4μg/L加标水样的回收率平均值范围在71%~115%之间,6次平行测定的RSD范围在3.3%~15.6%之间。

A rapid method was developed for the determination of 16 Polycyclic aromatic hydrocarbons(PAHs)in water by solid-phase microextraction(SPME)coupled with gas chromatography-triple quadrupole mass spectrometry,The type of SPME fiber,extraction time,extraction temperature and collision energy were optimized by experiments.The result shows that 100μm polydimethylsiloxane(PDMS)fiber was used in extraction temperature at 40℃for 40min,along with stirring at 350r/min,then desorbed for 6min at 280℃in the gas chromatograph injector port,and detected in the multi-reaction monitoring(MRM)mode by GC-MS/MS.The method showed a good linear relationship for 16 PAHs in the range of 0.2～4μg/L,the linear correlation coefficients were 0.9953～0.9995,and the limits of detection were 0.001～0.02μg/L with average recovery rate of 71%～115%and relative standard deviations(RSD)of 3.3%～15.2%(n=6)in 0.4μg/L concentration level.