Extraction and on-fiber derivatization of chlorophenols in leather by internally cooled solid phase microextraction

Journal of the Brazilian Chemical Society

Universidade do Estado de Santa Catarina, Joinville, Brazil¹  Silveira, Cristine D. de Souza¹  Merib, Josias¹  Universidade Federal de Santa Catarina, Florianópolis, Brazil¹  Instituto Nacional de Ciência e Tecnologia de Bioanalítica, Campinas, Brazil¹  Martendal, Edmar¹  Carasek, Eduardo¹ 

关键词: cold fiber SPME;    phenols;    leather;    gas chromatography-mass spectrometry;    experimental designs;   

DOI  :  10.1590/S0103-50532012001200012

学科分类：化学（综合）

来源: SciELO

【 摘 要 】

B> This study proposes a new analytical procedure based on an internally cooled solid phase microextraction technique (CF-SPME) combined with on-fiber derivatization and gas chromatography-selected ion monitoring-mass spectrometry (GC-SIM-MS) for the determination of phenols extracted directly from leather samples. The extraction and derivatization conditions were optimized using experimental designs, such as: extraction time and sample temperature of 5 min and 170 ºC, fiber recoat temperature of 20 ºC, and exposing the fiber to the headspace of 70 µL of bis(trimethylsylyl)trifluoro-acetamide derivatizing agent for 23 min. Detection limits ranging from 1.03 to 2.68 µg g-1 and relative standard deviation (RSD) lower than 15% (n = 5) were obtained. The recovery was studied at three concentration levels and excellent recoveries ranging from 64.5 to 92.3% were obtained.

【 授权许可】

Unknown