高级检索

    加速溶剂萃取-液相色谱法测定PM2.5中18种多环芳烃

    Determination of 18 Polycyclic Aromatic Hydrocarbons in PM2.5 by Liquid Chromatography with Accelerated Solvent Extraction

    • 摘要: 提出了加速溶剂萃取-液相色谱法测定德国GS标志认证的18种多环芳烃(PAHs)的方法。PM2.5样品经二氯甲烷-丙酮(1+1)混合液在100℃加速溶剂萃取5 min,循环2次。萃取液浓缩至约1 mL,氮吹至近干,用乙腈定容至1 mL。所得溶液以不同体积比的乙腈和水的混合液为流动相进行梯度洗脱,采用紫外检测器(UV)-荧光检测器(FLD)串联检测,其中UV (波长254 nm)测定苊烯,FLD两个波长通道分别测定苯并j荧蒽和其余16种PAHs。结果表明:18种PAHs的质量浓度均在0.02~1.00 mg·L-1内与对应的峰面积呈线性关系,检出限(3S/N)为0.005~0.018 mg·L-1。按标准加入法进行回收试验,回收率为83.3%~108%,测定值的相对标准偏差(n=5)为0.82%~5.2%。

       

      Abstract: A method was proposed for determination of 18 polycyclic aromatic hydrocarbons (PAHs) identified by GS in Germany by liquid chromatography (LC) with accelerated solvent extraction (ASE). The PM2.5 sample was extracted by ASE with a mixture of dichloromethane-acetone (1+1) at 100℃ for 5 min, with 2 cycle. The extract was concentrated to about 1 mL, then to near dryness by N2-blowing, and the residue was made its volume up to 1 mL with acetonitrile. The solution obtained was analyzed with ultraviolet (UV)-fluorescence (FLD) detector, with the mixture of acetonitrile and water in different volume ratios as mobile phase for gradient elution. Acenaphthylene (AcPy) was detected by UV (λ=254 nm), and benzoj fluoranthene (BkF) and the other 16 PAHs were respectively determined by two wavelength channels of FLD. As shown by the results, linear relationships between values of peak area and mass concentration of 18 PAHs were found in the same range of 0.02-1.00 mg·L-1, and detection limits (3S/N) ranged from 0.005 to 0.018 mg·L-1. Test for recovery was made by standard addition method, giving results in the range of 83.3%-108%, and RSDs (n=5) ranged from 0.82% to 5.2%.

       

    /

    返回文章
    返回