Simultaneous determination of six dialkylphosphates in urine by liquid chromatography tandem mass spectrometry

Dulaurent, Sylvain; Saint-Marcoux, Franck; Marquet, Pierre; Lachâtre, Gérard

doi:10.1016/j.jchromb.2005.12.012

Cited by 56 publications

(29 citation statements)

References 33 publications

(108 reference statements)

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“…Because absolute recoveries of DAPs in water differ from those in urine matrix (data not shown), pooled urine should be used for a matrix matched calibration curve. LOD and LOQ values are below or similar to those reported by De Alwis et al [14,15], who used solid-phase extraction and GC-MS/MS, Dulaurent et al [16], who used liquid-liquid extraction and LC-MS/MS, or by Ueyama et al [8]. Concentrations of LOQ are lower than the geometric mean of urinary DAPs in the general populations including children and pregnant women [12,[17][18][19], suggesting that our present method is sensitive enough for monitoring urinary DAPs in most general populations.…”

Section: Assay Validationsupporting

confidence: 54%

“…Moreover, the clean-up procedure after derivatization using a multi-layer column effectively removed the highly irritating PFBBr and other interfering substances, resulting in a drastic reduction of unidentifiable peaks in both the total ion chromatogram (TIC) and the selected ion monitoring (SIM) chromatograms, and stabilization of the baseline. Both GC-MS and LC-MS/MS methods have been developed to detect DAPs in urine [11,15,16], and these sophisticated analytical tools have inherent advantages in terms of high selectivity and sensitivity. The major advantage of the LC-MS/MS-based method is its ability to analyze various metabolites simultaneously with substantially simple sample pretreatment.…”

Section: Advantages Of This Methodsmentioning

confidence: 99%

“…However, these advantages are partially counterbalanced by the higher instrument cost in comparison with GC-MS systems. Moreover, sensitivity in DAP measurement using LC-MS/MS [15,16] at present tends to be lower than that using GC-MS or GC-MS/MS method [8,14,15]. In this study we combined the liquid-liquid extraction and GC-MS determination to achieve a lower-cost, faster and higher sample processing capacity.…”

Section: Advantages Of This Methodsmentioning

confidence: 99%

See 2 more Smart Citations

Revised method for routine determination of urinary dialkyl phosphates using gas chromatography–mass spectrometry

Ueyama

Kamijima

Kondo

et al. 2010

Journal of Chromatography B

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Section: Assay Validationsupporting

confidence: 54%

Section: Advantages Of This Methodsmentioning

confidence: 99%

Section: Advantages Of This Methodsmentioning

confidence: 99%

See 1 more Smart Citation

Revised method for routine determination of urinary dialkyl phosphates using gas chromatography–mass spectrometry

Ueyama

Kamijima

Kondo

et al. 2010

Journal of Chromatography B

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“…Dialkylphosphates, the major metabolites of OPs, have been determined in urine samples using gas chromatography (GC) [11,12], GC-MS [13][14][15], GC-MS-MS [16,17], and LC-MS-MS [18][19][20]. Their extraction procedures, however, are complicated and not specifi c for each OP [17].…”

Section: A Simple Methods For Detecting Fenitrothion Its Metabolite 3mentioning

confidence: 99%

A simple method for detecting fenitrothion, its metabolite 3-methyl-4-nitrophenol, and other organophosphorus pesticides in human urine by LC-MS

et al. 2008

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acute OP poisoning is most commonly encountered in emergency or forensic medicine [2,3]. The majority of such cases are attempts of suicide; in Japan, the OP compound most commonly used for this purpose is fenitrothion, followed by malathion and dichlorvos [4].Fenitrothion is categorized as a "moderately hazardous compound" (WHO class II) and is extensively used in many countries, including Japan, Canada, and Australia [3,5]. Although its oral toxicity in rats is low, fenitrothion poisoning is often life threatening or fatal in humans [6,7]. The authors have recently developed a rapid and reliable liquid chromatography-mass spectrometry (LC-MS) method for detection of OPs, including fenitrothion, in human serum [8], and have reported that serum fenitrothion concentration is useful in predicting the severity and outcome of fenitrothion poisoning [9]. OPs, however, are rapidly metabolized in the human body, suggesting that in most cases, the monitoring of parent compounds in blood is not reliable. In contrast, urinary concentrations of OPs and/or their metabolites are usually higher than the serum levels, and are probably detectable for longer periods of time [10].Dialkylphosphates, the major metabolites of OPs, have been determined in urine samples using gas chromatography (GC) [11,12], GC-MS [13-15], GC-MS-MS [16,17], and LC-MS-MS [18-20]. Their extraction procedures, however, are complicated and not specifi c for each OP [17].3-Methyl-4-nitrophenol (MNP) is a specifi c metabolite of fenitrothion. A method was developed for detection of both fenitrothion and MNP in serum and urine by high-performance liquid chromatography (HPLC) [21], but the validation of the analysis of fenitrothion and MNP has not been studied.Abstract A simple liquid chromatography-mass spectrometry (LC-MS) method was developed and carefully validated for quantitation of fenitrothion, its metabolite 3-methyl-4-nitrophenol, and fi ve other organophosphorus pesticides (acephate, cyanophos, methidathion, ethyl p-nitrophenyl phenylphosphonothioate, and malathion) in human urine samples. Following deproteinization by acetonitrile, the extracts were injected into an LC system and quantitated by MS in the negative ionization mode. The limits of detection were in the range of 0.25-0.75 μg/ ml for each analyte, and the method was validated on its accuracy and precision over the concentration range of 1-15 μg/ml. The method was successfully applied to an actual poisoning case and should prove useful in clinical and forensic toxicology.

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“…These DAP were among biomarkers of OP exposure used in epidemiology of children's environmental health (Wessels et al, 2003). They are suitable for biological monitoring of exposure to OP, and the determination of the alkylphosphate metabolites in urine is the most practical and widely used method to estimate the internal dose of most OP pesticides used worldwide (Angerer et al, 2007;Bouchard et al, 2006;Margariti & Tsatsakis., 2009;Dulaurent et al, 2006). However, it is necessary to understand the kinetics of metabolite excretion to know the optimum time for urine collection.…”

Section: Op Metabolitesmentioning

confidence: 99%

Biological Markers of Human Exposure to Pesticides

Araoud¹

2011

Pesticides in the Modern World - Pests Control and Pesticides Exposure and Toxicity Assessment

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Simultaneous determination of six dialkylphosphates in urine by liquid chromatography tandem mass spectrometry

Cited by 56 publications

References 33 publications

Revised method for routine determination of urinary dialkyl phosphates using gas chromatography–mass spectrometry

Revised method for routine determination of urinary dialkyl phosphates using gas chromatography–mass spectrometry

A simple method for detecting fenitrothion, its metabolite 3-methyl-4-nitrophenol, and other organophosphorus pesticides in human urine by LC-MS

Biological Markers of Human Exposure to Pesticides

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