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

崔世勇; 樊珠凤; 曹林波; 王硕; 景素芬

doi:10.19428/j.cnki.sjpm.2020.19587

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

摘要

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5 μg/L~200 μg/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。

Abstract:
ObjectiveTo 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).
MethodsThe 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 4 000 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.
ResultsGood linearities were obtained for the seven polycyclic aromatic hydrocarbons within the range of 5 μg/L-200 μg/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%.
ConclusionThe 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.

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