全二维气相色谱-质谱法定性分析土壤中有机氯农药、酞酸酯和多氯联苯

Qualitative analysis of organochlorine pesticides,phthalate esters and polychlorinated biphenyls in soil by comprehensive two-dimensional gas chromatography coupled to mass spectrometry

建立了土壤中20种有机氯农药、16种酞酸酯和18种多氯联苯的全二维气相色谱-质谱分离和定性方法。土壤样品与无水Na2SO4(1:1,m/m)混匀后,用丙酮、正己烷(1:1,V/V)在微波快速溶剂萃取仪上以1600W的功率,在20 min内从室温升至110℃,并保持20 min的条件进行萃取。通过优化升温速率、调制周期及热喷时间等参数,该方法能够在40.5 min内分离目标化合物及土壤萃取杂质,并通过二维谱图和质谱检索对54种目标化合物准确定性。

Comprehensive two-dimensional gas chromatography with mass spectrometry （ GC x GC-MS） has been applied to qualitative analysis of 20 organoehlorine pesticides, 16 phthalate esters and 18 polychlorinated biphenyls in soil. Samples mixed with anhydrous sodium sulfate （1：1 m/m ）were extracted with microwave extraction using a mixture of acetone and n-hexane （ 1 ： 1 V/V） under the following conditions ： 1600W, heating from room temperature to 110 ℃ within 20 rain and remaining 110 ℃ for 20 rain. After optimization of temperature program, modulation period, hot jet duration time and so on, all 54 compounds were separated from the soil matrix in 40. 5 min and identified accurately by GC x GC ehromatogram and mass spectrum.