三维石墨烯富集-GC-MS测定水样中16种邻苯二甲酸酯类化合物

Determination of 16 phthalate acid esters in water samples by GC-MS and three-dimensional graphene enrichment

目的建立一种同时检测大体积水样中16种邻苯二甲酸酯类化合物的三维石墨烯富集-气相色谱-质谱联用法。方法三维石墨烯富集大体积水样中邻苯二甲酸酯类化合物后,先用乙酸乙酯洗脱,然后用正己烷定容,再用HP-5MS气相色谱柱(30 m×0.25 mm,0.25μm)分离,通过质谱选择离子模式进行监测,以外标法定量。结果 16种酯类化合物的浓度为0.50 mg/L^50.0 mg/L时,其线性关系良好,线性相关系数(r)≥0.995,样品的加标回收率为81.81%~107.60%,相对标准偏差(RSD)为5.06%~10.00%,检出限为0.025 mg/L^0.050 mg/L。结论该方法前处理简便、快速、分析时间短、灵敏度高、重复性好,可用于大体积水样中16种酯类化合物的同时检测。

Objective To establish a method for simultaneous determination of 16 phthalate acid esters in water samples by gas chromatography- mass spectrometry（ GC- MS） after enriched with three dimensional（ 3D） graphene. Methods Phthalate acid esters component was enriched by 3D graphene,eluted with ethyl acetate,and quantified with n- hexane,and then separated with HP- 5MS column（ 30 m × 0. 25 mm,0. 25 μm）,and detected with mass spectrometer with SIM mode,as well as quantified with external reference method. Results The results showed a good linear correlation when the concentration of the16 phthalate acid esters was in the range of 0. 50 mg / L- 50. 0 mg / L,with the linear correlation coefficient（ r） greater than0. 995. The recoveries of the spiked sample were 81. 81%- 107. 60%,with the relative standard deviation（ RSD） of 5. 06%-10. 00%. The detection limit was 0. 025 mg / L- 0. 050 mg / L. Conclusion The pre- treatment of this method is simple,rapid,time- saving,sensitive and good repetative,which could be used for analyzing 16 phthalate acid esters in water samples.