聚硅氧烷改性聚乙二醇型聚氨酯固相微萃取膜的研制及其用于多环芳烃的测定  

Preparation of Solid Phase Microextraction Membrane of Polysiloxane Modified Polyethylene Glycol Polyurethane and Its Application for Determination of Polycyclic Aromatic Hydrocarbons

作　　者：申书昌[1] 刘艳萍[1] 任芳秀 

机构地区：[1]齐齐哈尔大学分析测试中心,齐齐哈尔161006

出　　处：《理化检验（化学分册）》2018年第2期130-137,共8页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：黑龙江省自然科学基金(B201101)

摘　　要：制成了聚硅氧烷改性聚乙二醇型聚氨酯固相微萃取膜,通过红外光谱和扫描电镜表征其结构及形貌。将固相微萃取膜与气相色谱法联用,测定了水中16种多环芳烃的含量。优化的试验条件如下:(1)萃取温度为35℃;(2)萃取时间为40min;(3)搅拌速率为400r·min^(-1);(4)10mL水样中氯化钠的加入量为1.5g。用HP-5毛细管色谱柱(30m×0.32mm,0.25μm)分离,火焰离子化检测器检测。16种多环芳烃的质量浓度均在0.05~5.0μg·L^(-1)内与其对应的峰高呈线性关系,方法的检出限(3S/N)为1.31~4.87ng·L^(-1),加标回收率为73.7%~102%,测定值的相对标准偏差(n=6)为5.4%~7.5%。Solid phase microextraction membrane of polysiloxane modified polyethylene glycol polyurethane was prepared. The structure and morphology were characterized by IR and SEM. GC was applied to the determination of 16 polycyclic aromatic hydrocarbons in the water with solid phase microextraction membrane. The optimized conditions found were as follows： （D extraction temperature was 35 ℃ ; （2） extraction time was 40 min; （3） stir speed was 400 r · min-1 ; （4） addition of NaCl in water sample （10 mL） was 1.5 g. The analytes were separated on HP-5 capillary chromatographic column （30 m×0. 32 mm, 0. 25μm） and detected by FID. Linear relationships between values of peak height and mass concentration of 16 polycyclic aromatic hydrocarbons were all kept in the same range of 0. 05-5.0 μg · L-1 , with detection limits （3S/N） in the range of 1.31-4.87 ng· L-1. Values of recovery found by standard addition method were in the range of 73.7 %- 102 %, and values of RSD＇s （n = 6） in the range of 5.4%--7.5%.

关 键 词：聚硅氧烷改性聚乙二醇型聚氨酯 固相微萃取膜 气相色谱法 多环芳烃 

分 类 号：O657.7[理学—分析化学]