Measurement of human urinary organophosphate pesticide metabolites by automated solid-phase extraction, post extraction derivatization, and gas chromatography–tandem mass spectrometry

Alwis, Gayani; Needham, Larry L.; Barr, Dana Boyd

doi:10.1016/j.jchromb.2006.05.010

Cited by 35 publications

(27 citation statements)

References 41 publications

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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: 66%

“…Previously, urinary DAPs have been extracted by various methods: liquid-liquid extraction [8,20,21], solid-phase extraction [14,15,22,23], and lyophilization [24]. Weerasekera et al [3] suggested that solid-phase extraction (ChemElute cartridge) and analysis using the GC-MS is the most cost-effective and rapid method.…”

Section: Advantages Of This Methodsmentioning

confidence: 99%

“…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%

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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: 66%

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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“…Nos Estados Unidos, de todos os praguicidas utilizados, os organofosforados representam 70% dos praguicidas comercializados. São praguicidas não somente utilizados na agricultura, mas também no controle de pragas residenciais (DE ALWIS;NEEDHAM;BARR, 2006) e em menor escala, no setor de saúde pública, com o objetivo de controlar e eliminar vetores de insetos causadores de doenças como a dengue e a malária (DE ALWIS;NEEDHAM;BARR, 2006).…”

Section: Outra Estimativa Da Organização Mundial Da Saúde E Da Organiunclassified

Avaliação da exposição ocupacional a praguicidas organofosforados em estufas de flores na região do Alto Tietê - São Paulo

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Measurement of human urinary organophosphate pesticide metabolites by automated solid-phase extraction, post extraction derivatization, and gas chromatography–tandem mass spectrometry

Cited by 35 publications

References 41 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

Avaliação da exposição ocupacional a praguicidas organofosforados em estufas de flores na região do Alto Tietê - São Paulo

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