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
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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:(1)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 0.05-5.0μg·L~(-1),with detection limits(3 S/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%.
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:(1)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 0.05-5.0μg·L~(-1),with detection limits(3 S/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%.
引文
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[16]申书昌,宋文成,贾鹏禹.硅氧烷-聚氨酯共聚物的制备及其作为固相微萃取头涂层用于分离水中芳香族化合物[J].理化检验-化学分册,2010,46(12):1444-1446.
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[19]刘保献,史鑫源,王小菊,等.气相色谱质谱法测定水质中16种多环芳烃[J].分析试验室,2015,34(7):827-831.
[2]傅若农.固相微萃取(SPME)近几年的发展[J].分析试验室,2015,34(5):602-620.
[3]BRUHEIM I,LIU X C,PAWLISZYN J.Thin-film microextraction[J].Analytical Chemistry,2003,75:1002-1010.
[4]BOYACI E,PAWLISZYN J.Micelle assisted thinfilm solid phase microextraction:A new approach for determination of quaternary ammonium compounds in environmental samples[J].Analytical Chemistry,2014,86:8916-8921.
[5]GRANDY J J,BOYACI E,PAWLISZYN J.Development of a carbon mesh supported thin film microextraction membrane as a means to lower the detectionlimits of benchtop and portable GC/MS instrumentation[J].Analytical Chemistry,2016,88:1760-1767.
[6]ANGEL R L,MIRNAGHI F S,PAWLISZYN J.Determination of cocaine and methadone in urine samples by thin-film solid-phase microextraction and direct analysisin real time(DART)coupled with tandem mass spectrometry[J].Analytical and Bioanalytical Chemistry,2013,405:9723-9727.
[7]BOYACI E,SPARHAM C,PAWLISZYN A.Thinfilm microextraction coupled to LC-ESI-MS/MS for determination of quaternary ammonium compounds in water samples[J].Analytical and Bioanalytical Chemistry,2014,406:409-420.
[8]KLOSKOWSKI A,PILARCZYK M.Membrane solid-phase microextractions a new concept of sorbent preparation[J].Analytical Chemistry,2009,81:7363-7367.
[9]MIRNAGHI F S,HEIN D,PAWLISZYN J.Thinfilm microextraction coupled with mass spectrometry and liquid chromatography-mass spectrometry[J].Chromatographia,2013,76:1215-1223.
[10]杨瑞琴,谢文林.新型固相微萃取膜及其在分析沙土中梯恩梯的应用[J].分析科学学报,2003,19(5):443-444.
[11]杨瑞琴,文平波.新型固相微萃取膜及其应用[J].公安大学学报,2003,1(1):9-11.
[12]杨瑞琴,谢文林.新型固相微萃取膜的制备及其在生物检材中毒物提取的应用[J].分析测试学报,2004,23(2):66-68.
[13]杨红丽,王翊如,庄峙厦,等.新型壳聚糖固相微萃取薄膜的研制及性能研究[J].光谱学与光谱分析,2006,26(1):11-14.
[14]李碧芳,胡玉玲,赖丛芳,等.自制聚二甲基硅氧烷/二乙烯基苯固相微萃取膜富集水样中邻苯二甲酸酯类化合物[J].中山大学学报(自然科学版),2004,43(6):121-127.
[15]张换换,李文飞,刘军海.有机硅改性聚氨酯的合成及应用[J].西部皮革,2010,32(11):44-46.
[16]申书昌,宋文成,贾鹏禹.硅氧烷-聚氨酯共聚物的制备及其作为固相微萃取头涂层用于分离水中芳香族化合物[J].理化检验-化学分册,2010,46(12):1444-1446.
[17]HJ 478-2009水质多环芳烃的测定[S].
[18]李荫,柳叶,孙晓伟,等.多环芳烃的样品前处理技术研究进展[J].环境化学,2015,34(8):1460-1469.
[19]刘保献,史鑫源,王小菊,等.气相色谱质谱法测定水质中16种多环芳烃[J].分析试验室,2015,34(7):827-831.