Determination of Perfluoro-octanoic Acid and Its Salts in Fluoro-paint by Gas-chromatography-Mass Spectrometry
摘 要
超声萃取技术萃取氟涂料中的全氟辛酸及其盐类物质,萃取液经固相萃取、浓缩后与乙酰化试剂反应,以全氟癸酸甲酯为内标物内标法进行定量测定.对气相色谱-质谱条件进行选择,方法的线性范围为1.0~1×105μg·L-1,相关系数为0.999 7,检出限为0.1 μg·L-1,在高低两种浓度水平(100 μg·L-1及1 000 μg·L-1 PFOA)进行精密度和回收率试验,所得相对标准偏差分别为4.24%和3.58%,回收率在86%~111%之间.
Abstract
Perfluoro-octanoic acid (PFOA) and its salts were extracted ultrasonically with methanol from the paint sample,and the extract was concentrated by passing through a silica gel column with a layer of anhydrous Na2SO4 (ca. 1 cm) over the silica gel. An aliquot of the sample solution was taken and derivatized with acetylchloride to give methyl ester of PFOA. Methyl ester of perfluorodecanoic acid was used as internal standard in the GC/MS determination. Analytical conditions of GC/MS were given in detail. Linearity range of the method was found from 1.0-1×105μg·L-1 (r=0.999 7),with detection limit of 0.1 μg·L-1. Tests for precision and recovery of the method were performed at concentration levels of 100 μg·L-1 and 1 000 μg·L-1 of PFOA,values of RSD′s (n=6) found were 4.24% and 3.58% respectively,and recovery obtained were in the range from 86% to 111%.
中图分类号 O657.63
所属栏目 工作简报
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收稿日期 2006/12/14
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备注王利兵(1967-),男,江苏南通人,研究员,博士,主要从事化学危险品安全性评价技术研究.
引用该论文: WANG Li-bing,Lv Gang,LIU Shao-cong,LIU Jun. Determination of Perfluoro-octanoic Acid and Its Salts in Fluoro-paint by Gas-chromatography-Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2008, 44(3): 228~230
王利兵,吕刚,刘绍从,刘军. 气相色谱-质谱法测定氟涂料中全氟辛酸及其盐类物质[J]. 理化检验-化学分册, 2008, 44(3): 228~230
被引情况:
【1】吴晓红,周宇艳,马明,孙明星,陈潜, "气相色谱-三重四极杆串联质谱法测定不粘锅涂层中全氟辛酸",理化检验-化学分册 50, 1027-1029(2014)
【2】于峰,贾科玲,李娇,杨箭,孙海, "固相萃取-气相色谱-质谱法测定纺织品中全氟辛烷磺酸盐",理化检验-化学分册 51, 176-179(2015)
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参考文献
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【3】Eriko Okochi,Tomoko Nishimaki-Mogami,Kazuhiro Suzuki,et al. Perfluorooctanoic acid,a peroxisome-proliferating hypolipidemic agent,dissociates apolipoprotein B48 from lipoprotein particles and decreases secretion of very low density lipoproteins by cultured rat hypatocytes[J]. Biochimica et Biophysica Acta,1999,1437:393-401.
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【6】John L Butenhoff,David W Gaylor,John A Moore,et al. Characterization of risk for general population exposure to perfluorooctanoate[J]. Regulatory Toxicology and Pharmacology,2004,39:363-380.
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【8】杨玉林,王宏,芮振荣,等.色谱法分析血浆中全氟辛酸[J].色谱,2002,20(1):66-68.
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