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.
作者
崔世勇
樊珠凤
曹林波
王硕
CUI Shi-yong;FAN Zhu-feng;CAO Lin-bo;WANG Shuo(Baoshan Center for Disease Control and Prevention,Shanghai 201901,China)
出处
《上海预防医学》
CAS
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)。
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
dispersive liquid-liquid microextraction based on solidification of floating organic droplet
gas chromatography-mass spectrometry
polycyclic aromatic hydrocarbons
water
作者简介
崔世勇,男,学士,主任技师,研究方向:理化检验,E-mail:sycui@sina.com。