Measurement of Paraquat in Serum by High-Performance Liquid Chromatography

Miller, Julian J.; Sanders, E.; Webb, D.B.

doi:10.1093/jat/3.1.1

Cited by 33 publications

(6 citation statements)

References 8 publications

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“…The use of a single-point calibration allows for higher throughput of samples compared with a full 5to 8-point calibration curve (19,21). The limit of quantitation, 0.1 rag/L, compared favorably with other reported HPLC methods (16)(17)(18)(19)(20)(21) and in most cases provides sufficient sensitivity for prognosis (4).…”

Section: Validation Of Hplc Methodsmentioning

confidence: 90%

“…Several techniques have been reported for the quantitation of paraquat in human biological fluids including radioimmunoassay (11), spectrophotometry (12)(13)(14), gas chromatography (15), high-performance liquid chromatography (HPLC) with ultraviolet detection (16)(17)(18)(19)(20)(21), and capillary electrophoresis (22). In this study, we report the validation of an HPLC method using ultraviolet spectrophotometric detection for the quantitation of paraquat in plasma and urine.…”

Section: Introductionmentioning

confidence: 99%

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A Detection Scheme for Paraquat Poisoning: Validation and a Five-Year Experience in Australia

Taylor

Salm

Pillans

2001

Journal of Analytical Toxicology

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We report the validation of a quantitative method for paraquat in plasma and urine using high-performance liquid chromatography (HPLC) with ultraviolet detection (260 nm). Furthermore, we illustrate the use of this method in the clinic (over five years), in conjunction with a qualitative urine paraquat screen. Urine or plasma sample (1 mL) preparation was performed in duplicate using C18 solid-phase extraction. Chromatographic separation was achieved on a Zorbax RX-Silica column (250 x 4.6-mm i.d.). The mobile phase consisted of 96% sodium chloride (5 g/L) and 4% acetonitrile (pH 2.2) pumped at 1.0 mL/min. Using a single-point calibration (1.0 mg/L), the method was found to be linear from 0.1 to 5.0 mg/L. The accuracy and imprecision of the method, over the linear range and for plasma and urine, were 94.7-104.9% and < 12.2%, respectively. The limit of quantitation for both matrices was 0.1 mg/L. The absolute recovery of paraquat from plasma and urine was 79.9 +/- 5.3% and 88.2 +/- 5.3%, respectively. From January 1995 to February 2000, 47 qualitative urine paraquat screens were requested throughout Australia. Nine screens were positive, and eight were confirmed to have paraquat present by our HPLC method. One sample was not analyzed by HPLC because the patient died prior to analysis. Thus, no false-positive results were reported for the qualitative urine screen. An additional 11 samples were referred for patients with positive screens from other sites for HPLC confirmation. The presence of paraquat was confirmed in nine of these samples. In conclusion, a qualitative urine screen combined with our validated HPLC confirmation is an effective protocol for assessing suspected cases of paraquat poisoning.

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Section: Validation Of Hplc Methodsmentioning

confidence: 90%

Section: Introductionmentioning

confidence: 99%

A Detection Scheme for Paraquat Poisoning: Validation and a Five-Year Experience in Australia

Taylor

Salm

Pillans

2001

Journal of Analytical Toxicology

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“…Their LOQs were 50 ng/mL with S/N 2/1 for both PQ and DQ with the same injection mode. As regards the sensitivities of derivated spectrophotometric methods (O'Haver, 1979;Fell et al, 1981;Jarvie et al, 1981;Fuke et al, 1992) and liquid chromatographic methods (Miller et al, 1979;Gill et al, 1983;Nakagiri et al, 1989;Ito, 1993), they varied from 50 to 500 ng/mL and required an injected sample volume a thousand-fold greater than that in CE. The coefficients of variation for the intra-and inter-day experiments were quite correct ( Table 2).…”

Section: Discussionmentioning

confidence: 99%

“…Sodium dithionite reaction allows qualitative detection of PQ and DQ in urine or gastric fluid (Berry and Grove, 1971;Yuen et al, 1967). For serum or urine spectrophotometric methods are used (Knepil, 1977;Tayama et al, 1991;Kesari et al, 1997) or derivated spectrophotometric methods (O'Haver, 1979;Fell et al, 1981;Jarvie et al, 1981;Fuke et al, 1992), chromatographic analysis-highperformance liquid chromatography (Miller et al, 1979;Gill et al, 1983;Nakagiri et al, 1989;Ito, 1993), gas chromatography (Martens and Heynfrickse, 1974;Kawase et al, 1984) or gas chromatography-mass spectrometric methods (Draflan et al, 1977), radioimmunologic assays (Levitt, 1979;Fatori and Hunter, 1980) and RMN 1 H (Imbenotte et al, 1999). Interest in capillary electrophoresis has greatly increased.…”

Section: Introductionmentioning

confidence: 99%

Separation and quantification of paraquat and diquat in serum and urine by capillary electrophoresis

Vinner

Stievenart

Humbert

et al. 2001

Biomedical Chromatography

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The use of capillary electrophoresis (CE) for simultaneous qualitative and quantitative detection of paraquat (PQ) and diquat (DQ) in both serum and urine was investigated. The two herbicides were extracted from biological fluids with liquefied phenol. Serum required a deproteinization with chloroform and ammonium sulfate as pretreatment. The extracts were hydrodynamically injected and the complete separation was carried out in 10 min, using a capillary tube (75 microm i.d., 500 mm) of fused silica containing 50 mM phosphate buffer (pH 2.50) as the carrier. UV absorbance detection at 200 nm was performed by an on-column detector. The analytes were characterized by their respective migration times. Analytical recoveries were 52.6% for PQ and 62.6% for DQ in serum, and 71.4% and 59.3%, respectively, in urine. The linearity was studied up to 4 mg/L and the limits of detection (LODs) were better than 5 pg/mL in serum or urine. The CE method described was applied to the characterization of two lethal poisonings and results were related.

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“…Most commercial products are available as a mixture of both compounds and therefore rapid methods capable of analyzing Pq and Dq separately and simultaneously in biological fluids are required by forensic and clinical examiners. Various analytical methods such as immunoassays (Niewola et al, 1985;Emon et al, 1986;Tomita et al, 1988) and spectrophotometric (Calderbank and Yuen, 1965;Berry and Grove, 1971;Jarvie and Stewart, 1979;Kuo, 1986) and chromatographic (Pryde and Darby, 1975;Draffan et al, 1977;Miller et al, 1979;Needham ef al., 1979) methods have been applied to the analysis of these herbicides, but few have considered the simultaneous microanalysis of both herbicides.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of paraquat and diquat in serum using capillary electrophoresis

Tomita

Okuyama

Nigo

1992

Biomedical Chromatography

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The use of capillary electrophoresis for simultaneous separation and detection of the two bipyridylium herbicides, paraquat and diquat, was investigated. Both herbicides were extracted from fortified sera with disposable ODS-silica cartridges. Separation was carried out using a capillary tube (50 microns i.d., 750 mm) of fused silica containing 10 mM glycine-HCl buffer (pH 3.0), 40 mM NaCl and 20% methanol as the carrier. Paraquat and diquat were completely separated in 10 min at an applied potential of 20 kV. On-column UV monitoring allowed detection of both herbicides simultaneously. The assay sensitivity was 0.05 micrograms/mL (signal-to-noise ratio, 2:1), which probably increases with increase in the sample volume of serum. Analytical recovery of both herbicides added to serum was about 97% at concentrations of 0.5-2.0 micrograms/mL.

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Measurement of Paraquat in Serum by High-Performance Liquid Chromatography

Cited by 33 publications

References 8 publications

A Detection Scheme for Paraquat Poisoning: Validation and a Five-Year Experience in Australia

A Detection Scheme for Paraquat Poisoning: Validation and a Five-Year Experience in Australia

Separation and quantification of paraquat and diquat in serum and urine by capillary electrophoresis

Simultaneous determination of paraquat and diquat in serum using capillary electrophoresis

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