超声提取-气相色谱-串联质谱法测定PM2.5中多环芳烃

Determination of Polycyclic Aromatic Hydrocarbons in Atmospheric Fine Particulate Matter by Gas Chromatography -Triple Quadrupole Mass Spectrometry with Ultrasonic Extraction

  • 摘要: 为满足小流量采样及复杂基质大气PM2.5中痕量多环芳烃的测定需求,建立了超声提取-气相色谱-串联质谱测定PM2.5中16种多环芳烃的方法,研究了离子源温度对测定和方法性能指标的影响,优化了碰撞电压,并通过对实际样品的测定,考察了方法的适应性。结果表明:PM2.5中16种多环芳烃在高、低浓度的标准曲线的线性关系良好,相关系数在0.995~0.999之间;方法的准确度和精密度较高,16种多环芳烃空白膜样品的加标回收率为84.4%~111%,实际样品的加标回收率为82.2%~95.3%,精密度均小于10%。当采样体积为24 m3时,各目标化合物的方法检出限为0.007 5~0.063 ng/m3。通过对多环芳烃浓度范围为0.04~1.04 ng/m3的夏季实际样品和0.2~30 ng/m3的冬季实际样品的检测分析,证明了本方法具有较低的检出限及较强的复杂基质抗干扰能力,能很好的满足PM2.5中多环芳烃的测定要求。

     

    Abstract: In order to meet the needs of determination of trace polycyclic aromatic hydrocarbons(PAHs) in PM2.5 with small flow sampling, a method of gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS) with ultrasonic extraction was established for the determination of 16 polycyclic aromatic hydrocarbons(PAHs) in PM2.5. The parameters were studied, like as the effect of different ion source temperature, the performance of the method, the collision voltage and the adaptability of this method by detecting the actual samples. Results show that the correlation coefficients of 16 PAHs in PM2.5 are 0.995-0.999. The recoveries of 16 PAHs are 84.4%-111% and 82.2%-95.3% for blank membrane samples and actual samples respectively, the precision is less than 10%. When the sampling volume is 24 m3,the limit detections of 16 PAHs are 0.007 5-0.063 ng/m3. Through the detection of the actual samples analysis (the concentration of PAHs ranged from 0.04-1.04 ng/m3 (in summer) and 0.2-30 ng/m3 in winter), the method has low detection limit and strong anti-interference ability with complex matrix, which can completely suitable for determination of PAHs in PM2.5.

     

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