Development of a solid phase microextraction-gas chromatography-mass spectrometry method for the determination of pentachlorophenol in human plasma using experimental design

作者：Zhou Ying; Jiang Qingwu; Peng Qian; Xuan Dongliang; Qu Weidong^*

来源：Chemosphere, 2007, 70(2): 256-262.

DOI：10.1016/j.chemosphere.2007.06.029

• SPME
• GC-MS
• Doehlert design
• central composite design
• pentachlorophenol
• human plasma

A new method, headspace solid-phase microextraction (HS-SPME) with in situ derivatization and gas chromatography-mass spectrometry (GC-MS), which was used for the determination of trace amount of pentachlorophenol (PCP) in human plasma was presented. The acetylation derivatization reaction was firstly optimized using a Doehlert design. Then a series of parameters relevant to the headspace SPME procedure, including fiber coating, extraction temperature, extraction time and salt addition, were optimized using a two-level full factorial design expanded further to a central composite design. The validation of method showed that the optimized method had good linearity (R-2 = 0.999) within the concentration ranges 0.1-50.0 ng ml(-1), and was sensitive with the limit of detection of 0.02 ng ml(-1). Intra- and inter-day precision for pentachlorophenol in human plasma samples were not greater than 11.9% and 12.6%, respectively. The proposed method, to our knowledge, describes the first application of HS-SPME with GC-MS for analysis of PCP in blood plasma sample. Application of the method to real human plasma samples, PCP was successfully detected in some cases at concentration levels 1.2-6.3 ng ml(-1).

• 出版日期2007-12
• 单位复旦大学