超声辅助乳化液液微萃取-气相色谱-质谱分析水中的人工合成麝香  

Determination of Synthetic Musks in Water by Ultrasound-assisted Emulsion Microextraction-Gas Chromatography-Mass Spectrometry

作　　者：虞锐鹏[1] 车金水[1] 何恩奇 钮伟民 宋启军[1] 王利平[1] 

机构地区：[1]江南大学食品科学与技术国家重点实验室,无锡214122 [2]无锡疾病预防控制中心,无锡214023

出　　处：《分析化学》2012年第1期159-163,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然基金(No.20977042);江苏省卫生厅科研基金项目(No.H200865);中国水产科学研究院重点开放实验室开放基金(No.YZ2009-05)

摘　　要：将超声辅助乳化与液液微萃取技术结合,建立了水体中人工合成麝香的气相色谱-质谱分析方法。优化前处理条件,包括萃取剂、萃取剂体积、萃取时间、萃取温度及离子强度的选择。结果表明:在10 mL水样中,加入50μL氯苯作为萃取剂,4 0 MHz超声10 min,混匀,以4000 r/min离心10 min,移取下层有机相进样分析,效果佳。样品的富集倍数可达200倍,8种人工合成麝香在0.005～0.4μg/L范围内线性关系良好,相关系数均大于0.994;检出限为0.3～0.5 ng/L;水样中加标回收率为96.2%～102.9%;相对标准偏差为2.3%～4.1%。本方法灵敏、快速、准确,可满足环境水样中痕量人工合成麝香监测的质控要求。A new analytical method,based on ultrasound-assisted emulsification technique,liquid-liquid microextraction,and gas chromatography/mass spectrometry（GC/MS）,was developed for the determination of eight synthetic musks in water samples.The pretreatment conditions,including the kind and volume of extraction solvent,extraction time,extraction temperature and ionic strength were studied.In this method,50 μL chlorobenzene as extraction solvent was added to 10 mL water sample,then ultrasonic for 10 min（40 MHz）,and centrifuged for 10 min（4000 r/min） to remove the organic phase for GC/MS analysis.Under the optimum separation and detection conditions,musks were confirmed and determined with internal standard method.The results show that enrichment factors for the samples were up to 200 times.The standard curves of 8 musks were linear in the concentration range of 0.005-0.4 μg/L with correlation coefficients of more than 0.994.The limits of detection were 0.3-0.5 ng/L,the recoveries were ranged from 96.2% to 102.9% and relative standard deviations were ranged from 2.3% to 4.1%.The method is rapid,simple,accurate,and was suitable for quanlitative confirmation and quantitative analysis of synthetic musk in environmental water samples.

关 键 词：水环境 人工合成麝香 超声辅助乳化液液微萃取 气相色谱-质谱联用 

分 类 号：O657.63[理学—分析化学] O661.1[理学—化学]