气相色谱-三重四级杆串联质谱法测定土壤中多环芳烃的方法研究

Determination of Polycyclic Aromatic Hydrocarbons in Soil by Gas Chromatography-triple Quadrupole Mass Spectrometry

[目的]建立索氏抽提、固相萃取净化、气相色谱-三重四极杆串联质谱法同时测定土壤及沉积物中16种多环芳烃(PAHs)的方法。[方法]对萃取、净化及仪器分析条件进行了优化。[结果]优化条件为:1+1的二氯甲烷+正己烷提取16 h,硅胶净化或不净化方法,PAHs浓度在0.25~5.00μg/mL时线性相关系数(R2)为0.990 3~0.999 9;PAHs方法检出限为0.002~0.020 mg/kg;加标回收率为61.2%~117.0%。[结论]试验结果为土壤中多环芳烃的测定提供了理论依据。

[Objective] The aim was to establish a method for the simultaneous extraction,cleanup,determination of 16 polycyclic aromatic hy-drocarbons （ PAHs） in soil by using Soxhlet extraction method and solid phase extration （ SPE） cleanup coupled with capollary gas chromatog-raphy-triple quadrupole mass spectrometry （GC-QqQ-MS/MS）.[Method] The conditions of extraction,cleanup,and instrumental operation were optimized.[Result] The optimal conditions of Soxhlet extraction method were extracted by dichloromethane＋n-hexane（1 ＋1） for 16 hours, and the Silicagel column was chosen as column of purification or nonpurification method was chosen.The correlation coefficient （R2） for PAHs were 0.9903-0.9999 in the range of 0.25 -5.00 μg/mL, and the limits of detection of PAHs were in the range of 0.002 -0.020 mg/kg;the recoveries of the samples ranged from 61.2%-117.0%.[Conclusion] The results provide reference for the determination of PAHs in soil.