超声提取-气相色谱-串联质谱法测定PM2.5中16种多环芳烃

Determination of 16 polycyclic aromatic hydrocarbons in PM2.5 by gas chromatograph-triple quadrupole mass spectrometry-ultrasonic extraction

目的建立大气PM2.5中16种多环芳烃(PAHs)的超声提取-气相色谱-串联质谱联用测定法。方法取1/8采样后的滤膜,剪碎后置于离心管中,加入10 ml正己烷浸没滤膜,15℃以下超声30 min,完成后5000 r/min离心5 min,取上清液5 ml氮吹至0.5 ml左右,正己烷准确定容至1 ml,GC-MS测定16种多环芳烃进行定性定量分析。结果该方法在1μg/L~100μg/L有良好的线性关系,相关系数为0.9992~0.9999,在多反应监测扫描模式下,在采样体积为144 m^(3)时检出限浓度为0.01 ng/m^(3)~0.10 ng/m^(3)。低、中、高浓度水平的空白样品平均加标回收率为62.7%~118.1%,相对标准偏差均<10%。结论该方法操作简便,灵敏度高,检出限低,抗干扰能力强,重现性好,定性定量更准确,适用于空气中16种多环芳烃的大批量检测。

Objective To establish a method for the determination of 16 kinds of polycyclic aromatic hydrocarbons(PAHs)in PM2.5 by ultrasonic extraction-gas chromatography-mass spectrometry(GC-MS/MS).Methods 1/8 of the sampled filter membrane was cut into pieces and placed in a centrifuge tube.10 ml ofn-hexane was added to soak the filter membrane and ultrasound was performed at 15℃for 30 minutes.After completion,centrifugation was performed at 5000 r/min for5 minutes.Sixteen PAHs were determined by GC-MS for qualitative and quantitative analysis.Results The method has a good linear relationship in the range of 1μg/L-100μg/L,with a correlation coefficient of 0.9992 to 0.9999,and a limit concentration of 0.01 ng/m^(3)-0.10 ng/m^(3)at the sampling volume of 144 m^(3).The average recoveries of blank samples at low,medium and high concentration levels were 62.7%-118.1%,and the relative standard deviations were less than 10%.Conclusion This method is easy to operate,has high sensitivity,low detection limit,strong anti-interference ability,good reproducibility and more accurate qualitative quantification.It is suitable for mass detection of 16 PAH in the air.