控温超声提取-气相色谱-三重四级杆质谱测定大气细颗粒物(PM_(2.5))中的多环芳烃

Determination of Polycyclic Aromatic Hydrocarbons in Atmospheric Fine Particulate Matter(PM_(2. 5)) by Gas Chromatography-Triple Quadrupole Mass Spectrometry with Temperature Controlled Ultrasonic Extraction

建立了控温超声提取-气相色谱三重四级杆质谱测定大气细颗粒物（ PM2.5）中多环芳烃（ Polycyclic aromatic hydrocarbon,PAHs）的分析方法。 PM2.5中的PAHs用二氯甲烷-正己烷（2：1, V/V）控温超声提取3次,每次提取20 min,气相色谱-串联质谱分析,得到16种PAHs和6种替代物的标准曲线线性关系良好,相关系数均大于0.99,16种PAHs的检出限范围为0.013~0.12μg/L。实验中还观察到PAHs在空白滤膜中有微量存在,回收率实验中得到6种替代物的回收率在58.7%~108.2%之间,16种PAHs的空白滤膜加标的平均回收率在88.3%~104.0%之间,相对标准偏差均低于9.0%,实际滤膜加标的平均回收率在77.3%~98.7%之间,相对标准偏差均低于6.0%,本方法能够满足实际大气样品的测定。

An analytical method was described for the determination of polycyclic aromatic hydrocarbons （ PAHs） in atmospheric fine particulate matter （ PM2. 5 ） by gas chromatography-triple quadrupole mass spectrometry with controlled temperature ultrasonic extraction. The PAHs in PM2. 5 were extracted 3 times and each was 20 min with a mixed solution of dichloromethane and n-hexane （ 2： 1 , V/V ） by controlling temperature, and analyzed by gas chromatography-triple quadrupole mass spectrometry. The results showed that 16 PAHs and 6 substitutes had good liner relationship, and the correlation coefficients were above 0. 99, the lowest detection limits for 16 PAHs were between 0. 013-0. 12 μg/L. PAHs were also detected in blank membrane, and the precision test shows that 6 substitutes recoveries range from 58. 7% to 108. 2%, the average recoveries in blank membrane of 16 PAHs were between 88 . 3%-104 . 0%, the relative standard deviationa of all PAHs are below 9 . 0% but actual membrane average recoveries are between 77 . 3%-98 . 7%, and the relative standard deviationa of all PAHs were below 6 . 0%. This method can meet the detection requirements for atmospheric samples.