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KMID : 0370220100540060429
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Yakhak Hoeji
2010 Volume.54 No. 6 p.429 ~ p.440
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Simultaneous Analysis of 17 Organophosphorous Pesticides in Blood by Automated Head Space-SPME GC/MS
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Lee Jong-Sook
Jung Jin-Mi
Lee Han-Sun
Yeom Hye-Sun
Lee Sang-Ki
Park Yoo-Shin
Chung Hee-Sun
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Abstract
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HS-SPME-GC/MS was studied and optimized for the determination of 17 orgarnophosphorous pesiticides (OPPs: chlorpyrifos, chlorpyrifos-methyl, demeton-s-methyl, diazinon, dimethoate, EPN, fenitrothion, fenthion, malathion, methidathion, monocrotophos, parathion, phenthoate, phosphamidon, sulfotep, terbufos, triazophos) in blood. Optimum SPME parameters were selected: choice of SPME fiber (85 polyacrylate), pH effect (0.5 N HCl), salt effect (, 0.2 g; 20%), headspace incubation temperature (), headspace incubation time (1 min), headspace adsorption time (30 min) and GC desorption time (2 min). These parameters were optimized using HS-SPME autosampler coupled with gas chromatography-mass spectrometry (GC-MS). Method validation was carried out in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ) and recovery in blood. The assay was linear over 0.5~5.0 mg/l (=0.955~1.000). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.03~0.3 mg/l (S/N=3) and 0.1~1.1 mg/l (S/N=10), respectively. Relative recovery with 0.5, 1 and 5 mg/l (in blood) were 90.8%, 98.5% and 94.1%, respectively. This method will be applied to the determination of the orgarnophosphorous pesticides in postmortem blood. The proposed protocol can be an attractive alternative to be used in routine toxicological analysis.
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KEYWORD
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pesiticide, HS-SPME-GC/MS, polyacrylate fiber, blood
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