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目的:建立了液液小体积超声萃取并结合气相色谱-质谱法检测水中16种邻苯二甲酸酯类化合物的方法。方法:运用萃取效率进行比较,选择了苯为最佳萃取试剂,并优化了苯的体积,盐的用量,超声时间等,当取样量为200 ml时,最终确定苯体积为2.0 ml,氯化钠加入20 g,超声50 min。结果:在优化的条件下,各组分的回收率在86.8%～111.2%之间,相对标准偏差范围为1.4%～12.5%,方法具有较高的灵敏度,方法检出限(信噪比(S/N)为3)为0.03μg/L～0.13μg/L。结论:该方法操作简便、快速、环境污染小,可用于水样中邻苯二甲酸酯类化合物的检测。
OBJECTIVE: To establish a method for the determination of 16 kinds of phthalates in water by ultrasonication and liquid chromatography-mass spectrometry. Methods: The extraction efficiency was used for the comparison. The optimal extraction reagent of benzene was selected and the volume of benzene, the amount of salt and ultrasonic time were optimized. When the sample volume was 200 ml, the final volume of benzene was 2.0 ml, Sodium was added to 20 g and sonicated for 50 min. Results: Under optimized conditions, the recoveries of the components ranged from 86.8% to 111.2%, and the relative standard deviations ranged from 1.4% to 12.5%. The method had high sensitivity and the detection limit (signal to noise ratio S / N) of 3) was 0.03 μg / L to 0.13 μg / L. Conclusion: The method is simple and rapid, and has low environmental pollution. It can be used for the determination of phthalates in water samples.