Development of a solid phase microextraction-gas chromatography-mass spectrometry method for the determination of pentachlorophenol in human plasma using experimental design.
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 0.1-50.0ngml(-1), and was sensitive with the limit of detection of 0.02ngml(-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 1.2-6.3ngml(-1).
School of Public Health, Fudan University, Shanghai 200032, People's Republic of China.
Ying
Y
Zhou
Qingwu
Q
Jiang
Qian
Q
Peng
Dongliang
D
Xuan
Weidong
W
Qu
D004785:Environmental Pollutants / Q000097:blood*; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D010416:Pentachlorophenol / Q000097:blood*; D012015:Reference Standards; D015203:Reproducibility of Results; D012107:Research Design; D012680:Sensitivity and Specificity; D052617:Solid Phase Microextraction
D004785:Environmental Pollutants; D010416:Pentachlorophenol