Rapid quantification of paraquat and diquat in serum and urine using high-performance liquid chromatography with automated sample pretreatment

Nakagiri, Itsuhiro; Suzuki, Kouichiro; Shiaku, Yumiko; Kuroda, Yasuhiro; Takasu, Nobuo; Kohama, Akitsugu

doi:10.1016/s0021-9673(01)96792-5

Cited by 22 publications

(9 citation statements)

References 8 publications

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“…[7][8][9][10] The best separation of PQ, DQ and IS was achieved on a Capcell Pak C18 UG120 reversed-phase column with methanol-200 mM phosphoric acid solution containing both 0.1 M diethyl amine and 12 mM sodium 1-heptane sulfonate (1:4, v/v) as an eluent. Figure 2 illustrates a typical chromatogram of a standard mixture of PQ, DQ and IS obtained with UV detection at 391 nm after the present postcolumn reductive reaction.…”

Section: Lc Separationmentioning

confidence: 99%

“…The sensitivity is approximately two times higher than those of the HPLC methods. [7][8][9][10] The sensitivity is sufficient for the assessment of the prognostic significance of the serum-PQ concentrations in poisoned patients.…”

Section: Precision and Accuracymentioning

confidence: 99%

“…21 min, which was twice or more times as rapid as those of HPLC methods. [7][8][9][10] The present HPLC method using a postcolumn reductive reaction requires only a deproteinization procedure for the simultaneous determination of the serum PQ and DQ. Postcolumn derivatization significantly improved the sensitivity and selectivity of this protocol.…”

Section: Validationmentioning

confidence: 99%

“…Several methods have been applied to simultaneously determine PQ and DQ serum levels; such methods are based on spectrophotometry, 3,4 gas chromatography (GC), 5,6 liquid chromatography (HPLC), [7][8][9][10] or capillary electrophoresis. 11 However, these methods have a limited sensitivity and/or specificity and require laborious and time-consuming sample preparation procedures such as cation-exchange chromatography, ion-pair liquid-liquid extraction and/or solidphase extraction.…”

Section: Introductionmentioning

confidence: 99%

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Rapid and Sensitive HPLC Method for the Simultaneous Determination of Paraquat and Diquat in Human Serum

et al. 2007

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A rapid and sensitive HPLC method for the simultaneous determination of paraquat and diquat in human serum has been developed. After deproteinization of the serum with 10% trichloroacetic acid, the samples were separated on a reversedphase column, and subsequently reduced to their radicals with alkaline sodium hydrosulfite solution. These radicals were monitored with a UV detector at 391 nm. This method permitted the reliable quantification of paraquat over linear ranges of 50 ng -10 μg/ml and 100 ng -10 μg/ml for diquat in human serum. The within-and between-day variations are lower than 2.3 and 2.2%, respectively. This technique was also utilized to determine the paraquat and diquat serum levels in a patient who had ingested herbicide (Prigrox L ® ) containing paraquat and diquat.

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Section: Lc Separationmentioning

confidence: 99%

Section: Precision and Accuracymentioning

confidence: 99%

Section: Validationmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Rapid and Sensitive HPLC Method for the Simultaneous Determination of Paraquat and Diquat in Human Serum

et al. 2007

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“…To the knowledge of the authors, a wide variety of methods have been reported for determining the serum level of paraquat or diquat, for example, thin-layer chromatography, 1) spectrochemical analysis, [2][3][4][5][6][7][8] HPLC, [9][10][11][12][13][14][15][16][17][18][19][20][21] LC/MS, 11) GC 22) and GC/MS. 23) In 1998, the Japanese Ministry of Health, Labor and Welfare distributed HPLC-photodiode array systems to 73 emergency centers throughout the country in order to facilitate the diagnosis of acute poisoning by drugs and poisons.…”

mentioning

confidence: 99%

Rapid Analysis Method for Paraquat and Diquat in the Serum Using Ion-Pair High-Performance Liquid Chromatography

Ito

Hori

Fujisawa

et al. 2005

Biological & Pharmaceutical Bulletin

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In acute poisoning by herbicides containing paraquat, or paraquat and diquat, it is possible to infer from the concentration of paraquat in the serum whether the patient will or will not survive, and this is of importance as a basis for deciding what approach to take in emergency treatment. In Japan, the main emergency medical centers where acute poisoning is a specialty have HPLC-photodiode array systems installed for the purpose of toxin analysis. However, in the conventional HPLC method, since it is necessary as a preliminary procedure to extract the paraquat and diquat from serum samples, analysis is time-consuming, and the establishment of a faster analytical technique is a significant step.To the knowledge of the authors, a wide variety of methods have been reported for determining the serum level of paraquat or diquat, for example, thin-layer chromatography, 1) spectrochemical analysis, 2-8) HPLC, 9-21) LC/MS, 11) GC 22) and GC/MS. 23) In 1998, the Japanese Ministry of Health, Labor and Welfare distributed HPLC-photodiode array systems to 73 emergency centers throughout the country in order to facilitate the diagnosis of acute poisoning by drugs and poisons. The application of these HPLC systems was a highly practical step. However, since the task of extraction from samples has to be carried out for the conventional methods reported for HPLC analysis of paraquat, the establishment of a faster technique of analysis would be useful in order to minimize delay in reaching a diagnosis of poisoning by a paraquat preparation.In the present study, after simply deproteinizing serum samples and introducing them directly to the HPLC column using an ion pair reagent as the mobile phase, we obtained good results with a new method that rapidly isolated and quantitated paraquat and diquat in an ODS column, and we report this and a number of cases in which analysis was actually performed. MATERIALS AND METHODS Reagents and Materials(1,1Ј-ethylene-2,2Ј-bipyridylium dibromide monohydrate) were purchased from Wako Pure Chemicals (Osaka, Japan), and ethyl viologen dibromide (1,1Ј-diethyl-4,4Ј-bipyridinium dibromide) was from Aldrich Chem. Co. (Milwaukee, WI, U.S.A.). These substances were dissolved in distilled water and were used as standard preparations. The ion-pair reagent IPCC-MS3 was purchased from GL Sciences Inc. (Tokyo, Japan). The distilled water was prepared by Wako Pure Chemicals (Osaka, Japan) for HPLC use, the acetone used was of special grade, and was manufactured by the same company, and the acetonitrile was a specially prepared reagent for HPLC produced by Nacalai Tesque, Inc. (Kyoto, Japan).Biological Specimen Collection Standard human serum for recovery tests was purchased from Sigma Chemical Co. (St. Louis, MO, U.S.A.), and was stored at Ϫ40°C until the time of analysis. The serum samples were derived from blood samples drawn from four patients poisoned by herbicides containing paraquat who ingested them with the aim of committing suicide and who were treated at the Emergency and Critical Care Center wher...

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Quantification of paraquat in postmortem samples by gas chromatography–ion trap mass spectrometry and review of the literature

Moreira

Pinho

Baltazar

et al. 2011

Biomedical Chromatography

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Paraquat (PQ) is an herbicide implicated in numerous fatalities, mainly caused by voluntary ingestion. Several methods have been used to quantify PQ in plasma and urine samples of intoxicated humans as a predictor of clinical outcome. There is no validated method for the analysis of PQ in postmortem samples. Therefore, the aim of this study was to develop an analytical method, using gas chromatography-ion trap mass spectrometry (GC-IT/MS) after solid-phase extraction, to quantify PQ in postmortem samples, namely in whole blood, urine, liver, lung and kidney, to cover the routes of distribution, accumulation and elimination of PQ. The method proved to be selective as there were no interferences of endogenous compounds with the same retention time as PQ and ethyl paraquat (internal standard). The regression analysis for PQ was linear in the range 0-10 µg/mL. The detection limits ranged from 0.0076 µg/mL for urine to 0.047 µg/mL for whole blood, and the recoveries were suitable for forensic analysis. The proposed GC-IT/MS method provided an accurate and simple assay with adequate precision and recovery for the quantification of PQ in postmortem samples. The proof of applicability was performed in two fatal PQ intoxications. A review of the analytical methods for the determination of quaternary ammonium herbicides is also provided for a better understanding of the presently available techniques.

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Rapid quantification of paraquat and diquat in serum and urine using high-performance liquid chromatography with automated sample pretreatment

Cited by 22 publications

References 8 publications

Rapid and Sensitive HPLC Method for the Simultaneous Determination of Paraquat and Diquat in Human Serum

Rapid and Sensitive HPLC Method for the Simultaneous Determination of Paraquat and Diquat in Human Serum

Rapid Analysis Method for Paraquat and Diquat in the Serum Using Ion-Pair High-Performance Liquid Chromatography

Quantification of paraquat in postmortem samples by gas chromatography–ion trap mass spectrometry and review of the literature

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