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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 three-dimensional graphene enrichment-gas chromatography-mass spectrometry (GC-MS) method for simultaneous determination of 16 phthalate esters in large volume of water samples. Methods After three-dimensional graphene was enriched in large volume of water samples, it was eluted with ethyl acetate and then fixed with n-hexane. The residue was chromatographed on a HP-5MS gas chromatographic column (30 m × 0.25 mm, 0.25 [mu] m), monitored by mass spectrometry with selected ion mode and quantified by external standard. Results When the concentration of 16 kinds of esters was 0.50 mg / L ~ 50.0 mg / L, the linearity was good, the linear correlation coefficient (r) was ≥0.995, the recoveries were 81.81% ~ 107.60%, the relative standard deviations (RSD) ranged from 5.06% to 10.00% with a detection limit of 0.025 mg / L to 0.050 mg / L. Conclusion The method is simple, rapid, short time, high sensitivity and reproducibility. It can be used for the simultaneous detection of 16 esters in a large volume of water samples.