建立了顶空固相微萃取与气相色谱法(HS-SPME-GC)测定人体尿液中五氯酚(PCP)的新方法.采用溶胶-凝胶法,加入自制的离子液体键合固相微萃取涂层,优化了萃取温度、萃取时间、pH值、离子强度及解吸时间.结果表明,样品中加入3 g NaCl,溶液的pH值为2,并以一定速度搅拌的条件下,在80℃顶空萃取50 min,300℃下解吸5min,方法的检测限为5.0 ng/L,线性范围为0.05～100μg/L,相对标准偏差(RSD)为5.9％,加标回收率为106.6％.
参考文献
| [1] | YANG Shuzhen,HAN Xiaodong,CHEN Wei.Advances in the Toxicity of Pentacholrophenol on Organism[J].Environ Health,2005,22 (5):396-398 (in Chinese).杨淑贞,韩晓冬,陈伟.五氯酚对生物体的毒性研究进展[J].环境与健康杂志,2005,22(5):396-398. |
| [2] | GUAN Wenna,XU Feng,LIAN Mei,et al.Preparation of Poly (trifluoropropyl) methylsiloxane Coating for Solid-Phase Micro-extraction and Its Application for the Analys of Phenolic Compounds in Sea Water[J].Chinese J Chromatogr,2007,25(5):614-618(in Chinese).观文娜,许峰,廉玫,等.聚甲基三氟丙基硅氧烷固相微萃取涂层的制备及其对海水中酚类化合物的分析[J].色谱,2007,25(5):614-618. |
| [3] | HE Qian,CHEN Jinfeng,LAI Dengyu,et al.Detemination of Phenols in Environmental Water by Solid Phase Microextraction Coupled with Gas Chromatography[J].Chinese J Anal Lab,2009,28(5):53-56(in Chinese).何茜,陈锦凤,赖登宇,等.SPME-GC联用测定环境水样中的酚类化合物[J].分析试验室,2009,28(5):53-56. |
| [4] | ZHOU Ruijuan,DUAN Lian,SUN Xiaojie,et al.IoIlic Liquid Bonded Coating Applied to Detemination of Pentachlorophenol in Water Sample by Solid-phase Micro-extraction Coupled with Gas Chromatography[J].Chem J Chinese Univ,2010,31:1945-1948 (in Chinese).周瑞娟,段炼,孙晓杰,等.离子液体键合固相微萃取涂层用于水样中五氯酚的测定[J].高等学校化学学报,2010,31:1945-1948. |
| [5] | ZHOU Ying,WU Xianfang,QU Weidong,et al.Study on the Method for Determination of Pentachlorophenol in Water[J].Hygiene Res,2007,36 (3):287-288 (in Chinese).周颖,吴显芳,屈卫东,等.水中五氯酚测定方法的研究[J].卫生研究,2007,36(3):287-288. |
| [6] | TANG Ting,WANG Hao,MA Wusheng,et al.Determination of Chlorophenols in Water by Derivatization Gas Chromatography[J].Chem Eng,2009,11:33-35 (in Chinese).汤颋,汪浩,马武生,等.衍生化气相色谱法测定水中的氯酚类[J].化学工程师,2009,11:33-35. |
| [7] | YAO Guiyan,GUAN Wenna,XU Feng,et al.Analysis of Phenolic Compounds in Aqueous Samples by Gas Chromatography Coupled with Headspace Solid-Phase Microextraction Using Poly (phthalazine ether sulfone ketone) Coated Fiber[J].Chinese J Chromatogr,2008,26 (5):590-594 (in Chinese).姚桂燕,观文娜,许峰,等.聚醚砜酮涂层纤维顶空固相微萃取-气相色谱法分析水中痕量的酚类化合物[J].色谱,2008,26(5):590-594. |
| [8] | TAI Changsong,ZHAO Ping,XU Xiaozuo,et al.Determination of Pentachlorophenol in Water by Headspace Solid Phase Microextraction Gas Chromatography[J].Environ Health,2004,21 (2):107-109 (in Chinese).邰昌松,赵萍,徐小作,等.水中五氯酚的顶空固相微萃取气相色谱测定法[J].环境与健康杂志,2004,21(2):107-109. |
| [9] | Brás I,Ratola N,Alves A.Uncertainty in the Quantification of Pentachlorophenol in Wood Processing Wastewaters by SPME-GC-MS[J].J Anal Chem,2011,66(8):756-762. |
| [10] | CAI Min,WANG Wei,XING Jun,et al.Direct Determination of Highly-substituted Chlorophenols Using a Novel Fiber by Solid-phase Microextraction[J].Chinese J Anal Chem,2006,34(1):91-94 (in Chinese).蔡敏,汪巍,邢钧,等.新型固相微萃取涂层直接检测样品中的3种多氯酚[J].分析化学,2006,34(1):91-94. |
| [11] | Huang M J,Tai C,Zhou Q F,et al.Preparation of Polyaniline Coating on a Stainless-steel Wire Using Electroplating and Its Application to the Determination of Six Aromatic Amines Using Headspace Solid-Phase Microextraction[J].J Chromatogr A,2004,1048(2):257-262. |
| [12] | Zhou Y,Jiang Q W,Peng Q,et al.Development of a Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry Method for the Determination of Pentachlorophenol in Human Plasma Using Experimental Design[J].Chemosphere,2007,70(2):256-262. |
| [13] | OUYANG Yunfu,TANG Hongbing,WU Ying,et al.Rapid Determination of Pentachlorophenol in Human Blood by Gas Chromatography with Headspace-Solid Phase Microextration[J].Chinese J Spectr Lab,2011,28 (2):627-630 (in Chinese).欧阳运富,唐宏兵,吴英,等.顶空固相微萃取气相色谱法快速测定人血中的五氯酚[J].光谱实验室,2011,28(2):627-630. |
| [14] | SUN Xiaojie,ZHANG Shaowen,WANG Fang,et al.Synthesis and Performance of Polymeric Ionic Liquid as Stationary Phase for Gas Chromatography[J].Chem J Chinese Univ,2009,30(7):1326-1328(in Chinese).孙晓杰,张少文,王芳,等.聚硅氧烷键合离子液体的合成及色谱性能[J].高等学校化学学报,2009,30(7):1326-1328. |
| [15] | WANG Peng,WANG Daxi,GAO Jinsen,et al.Simulation Calculation of Structure and IR Spectra of Alkylli-midazolium Chloroaluminates Molten Salts[J].Chem J Chinese Univ,2006,27 (8):1505-1508 (in Chinese).王鹏,王大喜,高金森,等.三氯化铝烷基氯化咪唑盐结构和红外光谱的模拟计算[J].高等学校化学学报,2006,27(8):1505-1508. |
| [16] | Eberlin M N,Silv R C.Faster and Simpler Determination of Chlorophenols in Water by Fiber Introduction Mass Spectrometry[J].Anal Chim Acta,2008,620(1/2):97-102. |
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