摘要
对比并优化3种液相微萃取模式：静态直接浸入法、动态直接浸入法和中空纤维膜法，并与气相色谱-质谱联用检测饮品中邻苯二甲酸酯类。静态直接浸入法以2．0μL甲苯-环己烷（3：1，V/V）混合溶剂微滴在500r／min转速下静态萃取40min，动态直接浸入法以2．0乩甲苯微滴在400r／min转速下，以1次／min的活塞抽打速率抽打25次，中空纤维膜法以20止辛醇在800r／min转速下萃取30min。3种方法检测水体中邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二正丁酯以及邻苯二甲酸丁基卞基酯的线性范围、相对标准偏差分别为0．50～500μg／L（3．01％～13．7％），0．10—10μg/L（17．3％～23．1％）及0．10—100μg／L（8．10％～15.5％）。应用于实际饮品中邻苯二甲酸酯类的测定，3种方法的回收率分别为89．5％～115．2％，70．6％～91．0％和91．5％～112．8％。
Three kinds of liquid-phase microextraction （LPME） methods, including static direct-immersed LPME （ SDI-LPME ）, dynamic direct-immersed LPME （ DDI-LPME ） and hollow fiber LPME （ HF-LPME ） coupled with gas chromatograph-mass spectrometry （GC-MS） for the determination of phthalic acid esters （PAEs） in drink were compared. The optimized conditions of the three kinds of method were as follows： for SDI-LPME, the samples were extracted with 2.0 μL of the mixture of toluene and cyclohexane（3：l, V/V） for 40 min at 500 r/min rotating speed; for DDI-LPME, the samples were extracted with 2.0 μL toluene at 400 r/min rotating speed and whipping 25 times at a rate of once a minute ; for HF-LPME, the samples were extracted with 20 μL octyl alcohol for 30 rain at 800 r/rain rotating speed. The linear ranges and the relative standard deviation of the three methods are 0. 50-500 μg/L（3.0% -13.7% ）, 0. 100-10.0 μg/L（ 17.3% - 23.1% ） and 0.100-100. 0 μg/L （8.1% -15.5 % ）, respectively, for the determination of dimethyl phthalate （DMP）, diethyl phthalate （DEP）, dibutyl phthalate （DBP） and butyl benzyl phthalate （BBP）, and the standard addition recoveries were 89.5% -115.2% , 70.6% -91.0% , 91. 5% -112.8% , respectively, in real drink sample analysis.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2013年第10期1582-1586,共5页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No.21107018)
教育部科学技术重点项目(No.212129)
广东省自然科学基金(No.S2012010008172)资助项目
关键词
液相微萃取
静态直接浸入液相微萃取
动态直接浸入液相微萃取
中空纤维膜液相微萃取
邻苯
二甲酸酯类
Liquid-phase microextraction
Static direct-immersed liquid-phase microextraction
Dynamicdirect-immersed liquid-phase microextraction
Hollow fiber liquid-phase microextraction
Phthalic acid esters
