论文部分内容阅读
目的建立气相色谱-质谱法测定药酒中15种邻苯二甲酸酯的残留量。方法样品经60℃水浴蒸发乙醇后进行固相分散萃取净化,采用DB-1701色谱柱分离;质谱采用电子轰击离子源(electron ionization,EI)模式电离,采用选择性离子检测(selected ion monitor,SIM)模式对15种邻苯二甲酸酯的定量离子和定性离子进行检测。比较了3种样品前处理方法对回收率的影响,同时对空白干扰问题进行了讨论。结果本方法在10 min内完成样品前处理,在30 min内完成对15种目标化合物的较好分离,15种邻苯二甲酸酯在0.5~8 mg/L范围内线性关系良好(r~2≥0.9991),在0.1、1.0和3.0μg/mL 3个添加水平上的回收率为88.0%~123.7%,相对标准偏差小于2.9%(n=6),检出限在0.002~0.04 mg/L之间。结论该方法操作简单准确,可适用于药酒中邻苯二甲酸酯的检测。
Objective To establish a GC-MS method for the determination of 15 phthalate residues in medicinal liquor. Methods The samples were purified by solid-phase dispersive extraction after ethanol was evaporated in a water bath at 60 ° C and separated on a DB-1701 column. Mass spectrometry ionization was performed using electron ionization (EI) mode with selected ion monitor (SIM) ) Mode to detect 15 kinds of phthalates quantitative ions and qualitative ions. The effects of three sample pretreatment methods on the recovery rate were compared. The blank interference problem was also discussed. Results The sample was pretreated in less than 10 min, and 15 target compounds were separated within 30 min. The linearity of 15 phthalates in the range of 0.5-8 mg / L was good (r ~ 2 ≥0.9991). The recoveries of the three addition levels at 0.1, 1.0 and 3.0 μg / mL ranged from 88.0% to 123.7% with relative standard deviations less than 2.9% (n = 6) and the limits of detection ranged from 0.002 to 0.04 mg / L between. Conclusion The method is simple and accurate and can be applied to the detection of phthalates in medicinal liquor.