A fatal dichlorvos poisoning: concentrations in biological specimens.
(2008)
Journal - Journal of forensic sciences (United States )
Abstract :
A 54-year-old man was found dead with a bottle containing a brownish fluid near him. A toxicological screening was carried out in blood, urine, and stomach content. Only dichlorvos (2,2 dichlorovinyl O-O dimethylphosphate or DDVP) was found. A simple and rapid method, using DDVP-D(6) as an internal standard, was developed for the determination of DDVP by gas chromatography/mass spectrometry (GC/MS). The method was linear from 1 to 10 mg/L. Intraday and interday precisions were all <15%. DDVP concentration in cardiac blood was approximately four times higher than in peripheral blood. A high concentration was found in the heart showing a cardiac tropism of DDVP, kidney and lung concentrations being much lower. No DDVP was found in liver. DDVP stomach content was 38 g. The amount presumed ingested was 82 g, c. 1000 mg/kg of body. The oral LD(50) for DDVP ranges between 20 and 1090 mg/kg in animals but is not known for humans.
| ISSN : | 1556-4029 |
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| Mesh Heading : | Dichlorvos Forensic Toxicology Gas Chromatography-Mass Spectrometry Gastrointestinal Contents Humans Insecticides Kidney Lung Male Middle Aged Molecular Structure Myocardium chemistry chemistry chemistry chemistry |
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| Mesh Heading Relevant : | analysis poisoning analysis poisoning |
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Sensitive quantification of apomorphine in human plasma using a LC-ESI-MS-MS method.
(2006)
Journal - Therapeutic drug monitoring (United States )
Abstract :
An analytical method based on liquid chromatography coupled with ion trap mass spectrometry (MS) detection with electrospray ionization interface has been developed for the identification and quantification of apomorphine in human plasma. Apomorphine was isolated from 0.5 mL of plasma using a liquid-liquid extraction with diethyl ether and boldine as internal standard, with satisfactory extraction recoveries. Analytes were separated on a 5-microm C18 Highpurity (Thermohypersil) column (150 mm x 2.1 mm I.D.) maintained at 30 degrees C, coupled to a precolumn (C18, 5-microm, 10 mm x 2.0 mm I.D., Thermo). The elution was achieved isocratically with a mobile phase of 2 mM NH4COOH buffer pH 3.8/acetonitrile (50/50, vol/vol) at a flow rate of 200 microL per minute. Data were collected either in full-scan MS mode at m/z 150 to 500 or in full-scan tandem mass spectrometry mode, selecting the [M+H]ion at m/z 268.0 for apomorphine and m/z 328.0 for boldine. The most intense daughter ion of apomorphine (m/z 237.1) and boldine (m/z 297.0) were used for quantification. Retention times were 2.03 and 2.11 minutes for boldine and apomorphine, respectively. Calibration curves were linear in the 0.025 to 20 ng/mL range. The limits of detection and quantification were 0.010 ng/mL and 0.025 ng/mL, respectively. Accuracy and precision of the assay were measured by analyzing 54 quality control samples for 3 days. At concentrations of 0.075, 1.5, and 15 ng/mL, intraday precisions were less than 10.1%, 5.3%, and 3.8%, and interday precisions were less than 4.8%, 6.6%, and 6.5%, respectively. Accuracies were in the 99.5 to 104.2% range. An example of a patient who was given 6 mg of apomorphine subcutaneously is shown, with concentrations of 14.1 ng/mL after 30 minutes and 0.20 ng/mL after 6 hours. The method described enables the unambiguous identification and quantification of apomorphine with very good sensitivity using only 0.5 mL of sample, and is very convenient for therapeutic drug monitoring and pharmacokinetic studies.
| ISSN : | 0163-4356 |
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| Mesh Heading : | Apomorphine Chromatography, High Pressure Liquid Dopamine Agonists Dose-Response Relationship, Drug Drug Monitoring Humans Parkinson Disease Reproducibility of Results Spectrometry, Mass, Electrospray Ionization therapeutic use therapeutic use drug therapy |
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| Mesh Heading Relevant : | blood blood methods |
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A novel LC-ESI-MS-MS method for sensitive quantification of colchicine in human plasma: application to two case reports.
(2006)
Journal - Journal of analytical toxicology (United States )
Abstract :
A novel method based upon liquid chromatography coupled to ion trap mass spectrometry (MS) detection with electrospray ionization interface has been developed for the identification and quantification of colchicine in plasma or whole blood. Colchicine was isolated from plasma using a liquid-liquid extraction with dichloromethane at pH 8.0 and embutramide as an internal standard, with satisfactory extraction recoveries. Solutes were separated on a 3-microm C18 Uptisphere (Interchim) column (150 x 2.0-mm i.d.) using acetonitrile/2 mM NH4COOH pH 3.8 buffer (50:50, v/v) as the mobile phase with a flow-rate of 200 microL/min. Data were collected either in full-scan MS mode at m/z 100-450 or in full-scan MS-MS mode, selecting the ion m/z 400.1 for colchicine and m/z 294.1 for embutramide. The most intense daughter ion of colchicine (m/z 358.1) and embutramide (m/z 207.9) were used for quantification. Retention times were 2.40 and 4.25 min for colchicine and embutramide, respectively. Calibration curves were linear in the 0.50-50 ng/mL range. The limits of detection and quantification were 0.05 ng/mL and 0.50 ng/mL, respectively. The intra- and interassay precisions were < 14%, and the intra- and interassay accuracies were in the 97-105.8% range at either 2 or 20 ng/mL. A fatal case of colchicine self-poisoning with a lethal blood concentration of 60 ng/mL and nonfatal case with a plasma sample collected very late (at least 36 h after the ingestion) are presented. The described method enables the unambiguous identification and quantification of colchicine with a very good sensitivity, using only 1 mL of sample.
| ISSN : | 0146-4760 |
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| Mesh Heading : | Adult Aged Chromatography, Liquid Colchicine Female Humans Male Reproducibility of Results Sensitivity and Specificity Spectrometry, Mass, Electrospray Ionization methods poisoning methods |
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| Mesh Heading Relevant : | blood |
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A rapid and sensitive high-performance liquid chromatography method for determination of embutramide (a Tanax or T61 component) in human blood with photodiode-array UV detection.
(2004)
Journal - Journal of analytical toxicology (United States )
Abstract :
Tanax or T61 is an euthanasia solution commonly used in veterinary medicine. Embutramide is one of the three components. In accidental intoxication, suicide, or suicide attempt, the determination of embutramide is needed to confirm the hypothesis of intoxication. Because the amount of sample is sometimes limited in forensic cases, a new rapid and sensitive high-performance liquid chromatography method using only 0.1 mL of blood has been developed with liquid-liquid extraction. The eluate was monitored with a photodiode-array detector with a fixed wavelength at 273 nm. The method provided extraction recoveries greater than 83%. The detection limit was 0.2 mg/L, and the limit of quantitation was 0.6 mg/L. The linearity of standards was excellent (r > 0.997). Intra- and interday precisions were acceptable with a coefficient of variation | ISSN : | 0146-4760 |
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| Mesh Heading : | Adult Amides Chromatography, High Pressure Liquid Drug Combinations Forensic Medicine Gas Chromatography-Mass Spectrometry Humans Injections, Intravenous Male Quaternary Ammonium Compounds Reproducibility of Results Sensitivity and Specificity Suicide Tetracaine administration & dosage instrumentation administration & dosage administration & dosage |
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| Mesh Heading Relevant : | blood poisoning methods methods poisoning poisoning |
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