悬浮固化分散液液微萃取-气相色谱-质谱法测定水中7种多环芳烃  

Determination of seven polycyclic aromatic hydrocarbons in water by dispersive liquid-liquid microextraction based on solidification of floating organic droplet with gas chromatography-mass spectrometry

作　　者：崔世勇[1] 樊珠凤[1] 曹林波[1] 王硕[1] CUI Shi-yong;FAN Zhu-feng;CAO Lin-bo;WANG Shuo(Baoshan Center for Disease Control and Prevention,Shanghai 201901,China)

机构地区：[1]上海市宝山区疾病预防控制中心,上海201901

出　　处：《上海预防医学》2021年第3期254-258,共5页Shanghai Journal of Preventive Medicine

基　　金：上海市宝山区科学技术委员会项目(16-E-37)。

摘　　要：【目的】建立水中7种多环芳烃的悬浮固化分散液液微萃取-气相色谱-质谱法(DLLME-SFO-GC-MS)。【方法】详细考察了悬浮固化分散液液微萃取的实验条件,以十二醇为萃取剂,甲醇为分散剂,在8%氯化钠条件下,涡旋1 min,4 000 r/min离心5 min,于冰浴中浸泡,待十二醇凝固后转移,室温融化后进行气相色谱-质谱分析。【结果】7种多环芳烃在5μg/L~200μg/L范围内线性良好,相关系数≥0.996,检出限为1.6 ng/L~3.2 ng/L,回收率在86.2%~105%,相对标准偏差为3.8%~9.4%。【结论】本法快速灵敏,操作简便,有机溶剂消耗少,对环境友好,可用于水中多环芳烃的快速测定。[Objective]To develop a new method for the simultaneous determination of seven polycyclic aromatic hydrocarbons(PAHs)in water by dispersive liquid-liquid microextraction based on solidification of floating organic droplet(DLLME-SFO)with gas chromatography-mass spectrometry(GC-MS).[Methods]The experimental conditions of DLLME-SFO were determined with dodecanol as extractant solvent,methanol as dispersive solvent,inonic strength increased by adding 8%NaCl.After vortexed for 1 min and centrifuged at 4000 r/min for 5 min,the water sample was cooled down in an ice bath till dodecanol became solid and formed a small ball.Then the solidified dodecanol phase was transferred,and directly detected by GC-MS method after it melted.[Results]Good linearities were obtained for the seven polycyclic aromatic hydrocarbons within the range of 5μg/L-200μg/L.The correlation coefficients were above 0.996.The detection limits ranged from 1.6 ng/L to 3.2 ng/L.The average recoveries ranged from 86.2%to 105%and the RSDs from 3.8%to 9.4%.[Conclusion]The method is sensitive,fast and simple.It has the advantage of little organic solvent consumption,which is friendly to environment and suitable for the detection of seven PAHs in water.

关 键 词：悬浮固化分散液液微萃取 气相色谱-质谱法 多环芳烃 水样 

分 类 号：R1[医药卫生—公共卫生与预防医学]