Journal of analytical toxicology (J ANAL TOXICOL)

Publications in this journal

• Article: An HPLC-HR-MS-MS Method for Identification of Anticoagulant Rodenticides in Blood.

  Jason E Schaff, Madeline A Montgomery
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  ABSTRACT: This paper presents a fully validated method for the qualitative identification of bromadiolone, brodifacoum, coumachlor, coumatetralyl, difenacoum and warfarin in whole blood specimens. Samples are protein precipitated with acetonitrile, processed via solid-phase extraction and analyzed by high-performance liquid chromatography with high resolution tandem mass spectrometric detection. Limits of detection were 10 ng/mL or better for all analytes.
  Journal of analytical toxicology 05/2013;
• Article: Segmental Hair Analysis after a Single Dose of Zolpidem: Comparison with a Previous Study.

  Xiaopei Cui, Ping Xiang, Jingshuo Zhang, Yan Shi, Baohua Shen, Min Shen
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  ABSTRACT: Hair is a useful aid and sometimes even the only matrix in the analytical strategy in drug-facilitated crime (DFC) investigations. In this novel study, segmental hair analysis was performed after a single 10 mg dose of zolpidem was given to 20 Chinese volunteers. Hair was collected 1 month after administration and was analyzed using ultra-high-pressure liquid chromatography/electrospray ionization tandem mass spectrometry. Zolpidem concentrations were found to be in the range of 135.0-554.6 pg/mg in the proximal 0-2 cm segments. These results were markedly different from those reported by Villain et al., who used volunteers administered equal doses of zolpidem. The analytical method used, as well as the volunteers' hair color, inter-individual variations such as metabolic capacity, hair growth rate, drug incorporation rates, physical state of the hair, age, gender, body weight, etc. and diffusion from sweat or other secretions are all factors that should be considered when interpreting the DFC results.
  Journal of analytical toxicology 05/2013;
• Article: Comparison of a New Cobinamide-Based Method to a Standard Laboratory Method for Measuring Cyanide in Human Blood.

  Robert Swezey, Walter Shinn, Carol Green, David R Drover, Gregory B Hammer, Scott R Schulman, Anne Zajicek, David A Jett, Gerry R Boss
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  ABSTRACT: Most hospital laboratories do not measure blood cyanide concentrations, and samples must be sent to reference laboratories. A simple method is needed for measuring cyanide in hospitals. The authors previously developed a method to quantify cyanide based on the high binding affinity of the vitamin B12 analog, cobinamide, for cyanide and a major spectral change observed for cyanide-bound cobinamide. This method is now validated in human blood, and the findings include a mean inter-assay accuracy of 99.1%, precision of 8.75% and a lower limit of quantification of 3.27 µM cyanide. The method was applied to blood samples from children treated with sodium nitroprusside and it yielded measurable results in 88 of 172 samples (51%), whereas the reference laboratory yielded results in only 19 samples (11%). In all 19 samples, the cobinamide-based method also yielded measurable results. The two methods showed reasonable agreement when analyzed by linear regression, but not when analyzed by a standard error of the estimate or paired t-test. Differences in results between the two methods may be because samples were assayed at different times on different sample types. The cobinamide-based method is applicable to human blood, and can be used in hospital laboratories and emergency rooms.
  Journal of analytical toxicology 05/2013;
• Article: Quantification of Total Thyroxine in Plasma from Xenopus laevis.

  L G Luna, K Coady, J R McFadden, D A Markham, M J Bartels
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  ABSTRACT: There is evidence that the endocrine systems of certain fish and wildlife can be affected by chemical contaminants, possibly resulting in developmental and reproductive problems. Perturbations in the hypothalamus-pituitary-thyroid (HPT) axis, in particular, can be detrimental during early development. Because the rate of amphibian metamorphosis is controlled by circulating thyroid hormones, tadpoles undergoing metamorphosis have been selected as relevant test organisms for evaluating the potential effects of a substance on the HPT axis in vertebrates. An indicative measure of HPT functioning in these assays is the concentration of the thyroid hormone, thyroxine (T4), in frog plasma. Therefore, there is a need for a validated method to measure T4 in plasma during amphibian metamorphosis. This study describes a method involving mixed-mode strong cation exchange solid-phase extraction (SPE) with ultrahigh-performance liquid chromatography and isotope dilution tandem mass spectrometry (UPLC-ID-MS-MS) to quantify total T4 in a small volume (10 µL) of plasma from Xenopus laevis (African clawed frog). The SPE procedure, together with MS detection, produced the required selectivity for the analysis of both T4 and the T4 internal standard. The limit of detection of the method was determined to be 0.2 ng/mL, whereas the lower limit of quantification was 0.5 ng/mL. The intra-day and inter-day precision values were less than ±5 and ±10%, respectively. Concentrations of total T4 in the plasma of X. laevis tadpoles at metamorphic peak were calculated to be 10.7 ± 0.8 ng/mL, which is comparable to the results from radioimmunoassay. This validated UPLC-ID-MS-MS method for the determination of total T4 in plasma has demonstrated good accuracy and precision, with low susceptibility to interferences with the utilization of multiple reaction monitoring and ID.
  Journal of analytical toxicology 04/2013;
• Article: Validation of a Novel Immunoassay for the Detection of Synthetic Cannabinoids and Metabolites in Urine Specimens.

  Amanda Arntson, Bill Ofsa, Denise Lancaster, John R Simon, Matthew McMullin, Barry Logan
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  ABSTRACT: Synthetic cannabinoid drugs do not cross react on traditional marijuana immunoassay tests, preventing their use in large scale drug screening programs. This paper describes the validation and performance characteristics of two enzyme linked immunosorbent assays designed to detect the use of two common synthetic cannabinoids in urine, JWH-018 and JWH-250. The JWH-018 assay has significant cross-reactivity with several synthetic cannabinoids and their metabolites, whereas the JWH-250 assay has limited cross-reactivity. The assays are calibrated at 5 ng/mL with the 5-OH metabolite of JWH-018 and the 4-OH metabolite of JWH-250. The method was validated with 114 urine samples for JHW-018 and 84 urine samples for JWH-250 and confirmed by using liquid chromatography tandem mass spectrometry, which tests for metabolites of JWH-018, JWH-019, JWH-073, JWH-250 and AM-2201. The accuracy was determined to be 98% with greater than 95% sensitivity and specificity for both assays.
  Journal of analytical toxicology 04/2013;
• Article: Identification of a New Metabolite of GHB: Gamma-Hydroxybutyric Acid Glucuronide.

  Ida Nymann Petersen, Christian Tortzen, Jesper Langgaard Kristensen, Daniel Sejer Pedersen, Torben Breindahl
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  ABSTRACT: Gamma-hydroxybutyric acid (GHB) is an important analyte in clinical and forensic toxicology with a narrow detection window of 3-6 h. In the search of improved detection methods, the existence in vivo of a glucuronated GHB metabolite (GHB-GLUC) was hypothesized. Chemically pure standards of GHB-GLUC and a deuterated analogue for chromatography were synthesized. Liquid chromatography and tandem mass spectrometry were used for targeted analysis in anonymous clinical urine samples (n = 50). GHB-GLUC was found in concentrations ranging from 0.11 to 5.0 µg/mL (mean: 1.3 ± 1.2 µg/mL). Thus far, this is the first report of a GHB glucuronide detected in biological samples. Given that glucuronides generally have longer half-life values than their corresponding free drugs, GHB-GLUC should theoretically be a biomarker of GHB intoxication. It is also proposed that the hitherto unexplained reports of elevated GHB concentrations in some biological samples, which has caused the setting of a relatively high cutoff value (10 µg/mL), represent total GHB measurements (sum of free GHB and actively chemically hydrolyzed GHB-GLUC). To address these challenges, the present study must be followed by comprehensive pharmacokinetic and stability studies after the controlled administration of GHB.
  Journal of analytical toxicology 04/2013;
• Article: Prescription Opioids. I. Metabolism and Excretion Patterns of Oxycodone in Urine Following Controlled Single Dose Administration.

  Edward J Cone, Rebecca Heltsley, David L Black, John M Mitchell, Charles P Lodico, Ronald R Flegel
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  ABSTRACT: The ongoing epidemic of prescription opioid abuse in the United States has prompted interest in semi-synthetic opioids in the federal workplace drug testing program. This study characterized the metabolism and disposition of oxycodone (OC) in human urine. Twelve healthy adults were administered a single oral 20 mg dose of OC in a controlled clinical setting. Urine specimens were collected at timed intervals up to 52 h and analyzed by liquid chromatography-tandem mass spectrometry (limit of quantitation: 50 ng/mL) for OC, oxymorphone (OM), noroxycodone (NOC) and noroxymorphone (NOM) with and without enzymatic hydrolysis. OC and NOC appeared in urine within 2 h, followed by OM and NOM. Peak concentrations of OC and metabolites occurred between 3 and 19 h. Mean peak concentrations in hydrolyzed urine were in the following order: NOC > OC > OM > NOM. Only OM appeared to be excreted extensively as a conjugated metabolite. OC concentrations declined more quickly than NOC and OM. At a cutoff concentration of 50 ng/mL, detection times were approximately 30 h for OC and 40 h for NOC and OM. Some specimens did not contain OC, but most contained NOC, thereby facilitating interpretation that OC was the administered drug; however, five specimens contained only OM. These data provide information that should facilitate the selection of appropriate test parameters for OC in urine and assist in the interpretation of test results.
  Journal of analytical toxicology 04/2013;
• Article: Serial Ricinine Levels in Serum and Urine after Ricin Intoxication.

  Bent Tore Røen, Aase Mari Opstad, Anniken Haavind, Janne Tønsager
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  ABSTRACT: Ricinine is an alkaloid present in the castor bean plant (Ricinus communis) that can be used as a biomarker for ricin poisoning. Serial ricinine levels are reported in the serum and urine of a patient suffering from intentional ricin intoxication. The patient was brought to the hospital 4 h after injection and oral intake of a castor bean extract, but died 38 h later, despite intensive medical care. Ricinine was isolated from the samples by solid-phase extraction and quantitatively determined by isotopic dilution liquid chromatography-mass spectrometry. The ricinine level in serum declined from 33 to 23 ng/mL between 10 and 29 h post-exposure. Three urine samples collected from 12 to 41 h after ricin intoxication showed ricinine concentrations in the range of 20-58 ng/mL. The creatinine corrected values (21-30 µg/g) indicated a concentration-time profile with a maximum ricinine level in urine between 12 and 29 h after exposure.
  Journal of analytical toxicology 04/2013;
• Article: Gas and Liquid Chromatography-Mass Spectrometry Detection of the Urinary Metabolites of UR-144 and Its Major Pyrolysis Product.

  Andrej Grigoryev, Pierce Kavanagh, Alexandra Melnik, Sergey Savchuk, Anton Simonov
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  ABSTRACT: Studies on the pyrolysis of the synthetic cannabinoid agonist UR-144 ((1-pentyl-1H-indol-3-yl)(2,2,3,3-tetramethylcyclopropyl)methanone) have shown that its major pyrolysis product is a tetramethylcyclopropane ring-opened alkene. Considering that smoking is a common way of ingesting synthetic cannabimimetics, the presence of the metabolites of this pyrolysis product would be expected in biological fluids. Using GC-MS and LC-MS-MS methods, a series of phase I metabolites of UR-144 and its pyrolysis product were detected in the urine samples from patients admitted to hospital with suspected drug intoxication. The metabolites were tentatively identified as the products of mono-hydroxylation, di-hydroxylation, mono-hydroxylation with formation of the carbonyl group on the N-alkyl chain, carboxylation and N-dealkylation with mono-hydroxylation. In the case of the UR-144 pyrolysis product, metabolites with hydration of the aliphatic double bond were also identified. The parent compounds were detected as trace amounts in some urine samples, and the hydrated derivative of the UR-144 pyrolysis product was detected in the majority of samples. The detection of mono-hydroxylated metabolites of UR-144 (LC-MS-MS) and mono-hydroxylated/with hydration metabolites of the UR-144 pyrolysis product (GC-MS) was found to be the most useful method of establishing UR-144 ingestion.
  Journal of analytical toxicology 04/2013;
• Article: Swift Onset of Central Nervous System Depression and Asystole Following an Overdose of Guaifenesin.

  Merisa Okic, Tom Johnson, Joseph A Crifasi, Christopher Long, Erik K Mitchell
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  ABSTRACT: Guaifenesin is an over-the-counter expectorant used for chest congestion and is available both in single-ingredient formulations and in combination with antihistamines, cough suppressants and decongestants. The documented side-effects of guaifenesin are generally mild. We present the case of a 23-year-old female who committed suicide by ingestion of guaifenesin along with small amounts of cetirizine, ethanol and sertraline. Approximately 2 h after ingestion, the patient experienced central nervous system depression followed by asystole. No anatomic cause of death could be determined at autopsy. The initial toxicology detected only ethanol, which was found at a concentration insufficient to cause death. Upon further analysis, guaifenesin was detected in femoral blood at 25.0 μg/mL, urine at >50.0 μg/mL, vitreous fluid at 9.2 μg/mL, brain at 17.0 μg/g and liver at 25.0 μg/g. This is the first reported human case that can be considered a death to which guaifenesin was the significant pharmacologic contributor. Guaifenesin is not detected by the primary screening methods employed by some labs and may be missed in toxicological analyses of overdoses unless specifically suspected.
  Journal of analytical toxicology 04/2013;
• Article: Analysis of MDPV in Blood--Determination and Interpretation.

  Piotr Adamowicz, Dominika Gil, Agnieszka Skulska, Bogdan Tokarczyk
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  ABSTRACT: 3,4-Methylenedioxypyrovalerone (MDPV) is a cathinone derivative. It has recently been classified as a controlled substance in many countries. This substance is a stimulant that can be snorted, smoked or taken orally. MDPV has been determined in biological material from four cases sent to the Institute of Forensic Research in 2011. In the first case, a passenger car crashed into a truck; the driver of the vehicle suffered severe injuries, resulting in his death. In the second case, biological material was obtained from the decedent male individual, who did not wake up after a party. In the two cases, the material was secured on suspicion of the possession of narcotic drugs or psychotropic substances, in which the suspects admitted to using "legal highs." The MDPV blood concentrations of the deceased driver and deceased man were 38 and 17 ng/mL, respectively. In the two other cases, the determined concentrations were 306 and 124 ng/mL. However, MDPV was not the sole substance detected in these cases: in each, other drugs were also determined. Analyses of blood were conducted using liquid chromatography-tandem mass spectrometry.
  Journal of analytical toxicology 04/2013;
• Article: Field Testing of the Alere DDS2 Mobile Test System for Drugs in Oral Fluid.

  Christine Moore, Tara Kelley-Baker, John Lacey
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  ABSTRACT: A preliminary field evaluation of a second-generation handheld oral fluid testing device, the Alere DDS2 Mobile Test System (DDS2), is described. As part of a larger study, drivers were randomly stopped at various locations across California (in 2012) and asked to submit voluntarily to a questionnaire regarding their drug and alcohol use, a breath alcohol test and collection of oral fluid with the Quantisal device. The Quantisal-collected oral fluid samples were sent for laboratory-based analyses. At one location, 50 drivers were asked to submit an additional oral fluid sample using the DDS2 collection device; these samples were analyzed by using the DDS2 mobile test system. Thirty-eight donors (76%) provided specimens that were successfully run on the mobile system; in 12 cases (24%), the device failed to provide a valid result. Thirty-two of the 38 collected samples were negative for all drugs; five were positive for tetrahydrocannabinol and one was positive for methamphetamine using the mobile device. These results corresponded exactly with the laboratory-based results from the Quantisal oral fluid collection.
  Journal of analytical toxicology 04/2013;
• Article: From the Street to the Laboratory: Analytical Profiles of Methoxetamine, 3-Methoxyeticyclidine and 3-Methoxyphencyclidine and their Determination in Three Biological Matrices.

  Giorgia De Paoli, Simon D Brandt, Jason Wallach, Roland P Archer, Derrick J Pounder
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  ABSTRACT: Three psychoactive arylcyclohexylamines, advertised as "research chemicals," were obtained from an online retailer and characterized by gas chromatography ion trap electron and chemical ionization mass spectrometry, nuclear magnetic resonance spectroscopy and diode array detection. The three phencyclidines were identified as 2-(ethylamino)-2-(3-methoxyphenyl)cyclohexanone (methoxetamine), N-ethyl-1-(3-methoxyphenyl)cyclohexanamine and 1-[1-(3-methoxyphenyl)cyclohexyl]piperidine. A qualitative/quantitative method of analysis was developed and validated using liquid chromatography (HPLC) electrospray tandem mass spectrometry and ultraviolet (UV) detection for the determination of these compounds in blood, urine and vitreous humor. HPLC-UV proved to be a robust, accurate and precise method for the qualitative and quantitative analysis of these substances in biological fluids (0.16-5.0 mg/L), whereas the mass spectrometer was useful as a confirmatory tool.
  Journal of analytical toxicology 04/2013;
• Article: Analysis of Sertraline in Postmortem Fluids and Tissues in 11 Aviation Accident Victims.

  Russell J Lewis, Mike K Angier, Kelly S Williamson, Robert D Johnson
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  ABSTRACT: Sertraline (Zoloft) is a selective serotonin reuptake inhibitor that is a commonly prescribed drug for the treatment of depression, obsessive-compulsive disorder, panic disorder, social anxiety disorder, premenstrual dysphoric disorder and post-traumatic stress disorder. Although the use of sertraline is relatively safe, certain side effects may negatively affect a pilot's performance and become a factor in an aviation accident. The authors' laboratory investigated the distribution of sertraline and its primary metabolite, desmethylsertraline, in various postmortem tissues and fluids obtained from 11 fatal aviation accident cases between 2001 and 2004. Eleven specimen types were analyzed for each case, including blood, urine, vitreous humor, liver, lung, kidney, spleen, muscle, brain, heart and bile. Human specimens were processed utilizing solid-phase extraction, followed by characterization and quantitation employing gas chromatography-mass spectrometry. Whole blood sertraline concentrations obtained from these 11 cases ranged from 0.005 to 0.392 µg/mL. The distribution coefficients of sertraline, expressed as specimen/blood ratio, were as follows: urine, 0.47 ± 0.39 (n = 6); vitreous humor, 0.02 ± 0.01 (n = 4); liver, 74 ± 59 (n = 11); lung, 67 ± 45 (n = 11); kidney, 7.4 ± 5 (n = 11); spleen, 46 ± 45 (n = 10); muscle, 2.1 ± 1.3 (n = 8); brain, 22 ± 14 (n = 10); heart, 9 ± 7 (n = 11); and bile, 36 ± 26 (n = 8). Postmortem distribution coefficients obtained for sertraline had coefficients of variation ranging from 47-99%. This study suggests that sertraline likely undergoes significant postmortem redistribution.
  Journal of analytical toxicology 03/2013;
• Article: Quantitation of Urinary Volatile Nitrosamines from Exposure to Tobacco Smoke.

  Tiffany H Seyler, Jenny G Kim, James A Hodgson, Elizabeth A Cowan, Benjamin C Blount, Lanqing Wang
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  ABSTRACT: A sensitive and selective method was developed and validated to detect six volatile nitrosamines (N-nitrosodimethylamine, N-nitrosomethylethylamine, N-nitrosodiethylamine, N-nitrosopiperidine, N-nitrosopyrrolidine and N-nitrosomorpholine) in human urine. This method uses a liquid-liquid extraction cartridge followed by analysis with gas chromatography-tandem mass spectrometry (GC-MS-MS) and quantification based on isotopic dilution. This is the first GC-MS-MS method reported for measuring volatile nitrosamines in human urine. This method reduces the sample volume required in other methods from 5-25 to 2 mL. The limits of detection (2.62, 1.99, 2.73, 0.65, 0.25, 3.66 pg/mL, respectively) were better than existing methods, largely because of improved positive chemical ionization achieved by using ammonia gas and reducing background noise. Using nitrogen as the collision gas allowed the confirmation transition in the low mass region to be monitored. The analysis of human urine using this validated method is accurate (relative bias of 0-19%) and precise (relative standard deviation of 0.2-18% over two months of analyses). The validated method was applied to 100 urine samples and the levels of all six volatile nitrosamines were reported for the first time in urine specimens collected from smokers and nonsmokers, with smoking status determined by urinary cotinine measurement. Among 100 smokers and nonsmokers, the levels of three analytes (N-nitrosodimethylamine, N-nitrosomethylethylamine and N-nitrosopiperidine) were significantly higher in smokers than nonsmokers (p < 0.05).
  Journal of analytical toxicology 03/2013;
• Article: Uptake of Gamma-Valerolactone--Detection of Gamma-Hydroxyvaleric Acid in Human Urine Samples.

  H Andresen-Streichert, H Jungen, A Gehl, A Müller, S Iwersen-Bergmann
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  ABSTRACT: Gamma-valerolactone (GVL) is reported to be a substance that can be used as a legal substitute for gamma-hydroxybutyric acid (GHB), which is currently a controlled substance in several countries. Unlike gamma-butyrolactone and 1,4-butanediol, GVL is not metabolized to GHB, which causes the effects after uptake of these two chemicals. In the case of GVL, the lactone ring is split to gamma-hydroxyvaleric acid (GHV or 4-methyl-GHB) by a lactonase. Because of its affinity for the GHB receptor, GHV reveals similar effects to GHB, although it is less potent. Intoxications with GVL, or its use as a date rape drug, are conceivable. Despite these facts, there are no publications in the literature regarding detections of GHV in human samples. This study reports three cases, including five urine samples, in which GHV could be detected in concentrations between 3 and 5.8 mg/L. In one of these cases, a drug-facilitated sexual assault (DFSA) was assumed; four of these samples were from two people suspected of abusing GHB. The results indicate that GVL is used as an alternative to GHB and its precursors and should be taken seriously. GVL or GHV should be included in toxicological analysis, particularly in DFSA cases. More information is needed regarding the pharmacokinetics of GVL/GHV for the meaningful interpretation of positive or negative results.
  Journal of analytical toxicology 03/2013;
• Article: In Vitro Absorption of Atmospheric Carbon Monoxide and Hydrogen Cyanide in Undisturbed Pooled Blood.

  Tiffany M Thoren, Kristi S Thompson, Patrick S Cardona, Arvind K Chaturvedi, Dennis V Canfield
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  ABSTRACT: Blood samples from aircraft accident victims are analyzed for carboxyhemoglobin (COHb) and cyanide ion (CN-). Such victims often suffer open wounds near the autopsy blood collection sites. Many aircraft crashes result in fires that fill the victim's atmosphere with smoke that is rich in carbon monoxide (CO) and hydrogen cyanide (HCN). It is important to determine whether pooled blood in those wounds may have absorbed these gases after death, which could lead one to erroneously conclude that the presence of COHb and CN- in blood was the result of breathing in these gases. A laboratory desiccator was used as a chamber to establish whether CO or HCN may be absorbed in undisturbed, pooled blood. COHb levels were 4.3-11.0% after exposure to CO (5,532, 8,298, 11,064, 22,129 and 33,193 ppm) for 30 and 60 min. Blood CN- concentrations (1.43-5.01 µg/mL) increased with exposure to HCN at 100 and 200 ppm, each at 15, 30, 45 and 60 min. The observed COHb increases do not exclude the possibility for higher COHb levels in blood exposed to highly CO-rich atmospheres, but there is a strong potential for CN- levels to increase by the absorption of atmospheric HCN. Thus, postmortem COHb and CN- levels should be carefully interpreted.
  Journal of analytical toxicology 03/2013;
• Article: Rapid Immunoassay Method for the Determination of Clenbuterol and Salbutamol in Blood.

  J Pleadin, A Vulic, N Persi, S Terzic, M Andrisic, I Zarkovic
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  ABSTRACT: The aim of the study was to evaluate the adequacy of enzyme-linked immunosorbent assay (ELISA) in the post-exposure determination of the β-agonists clenbuterol and salbutamol in animal plasma and serum. Experimental guinea pigs (n = 20) were treated with two doses (0.25 and 2.5 mg/kg) of clenbuterol (n = 10) and salbutamol (n = 10) for seven days, whereas the control animal group (n = 10) was left untreated. Validation of the applied method yielded acceptable recovery (mean > 70%) and repeatability rates, showing ELISA to be applicable for the semi-quantitative determination of both analytes in both matrices, preferably in plasma. In both matrices, clenbuterol concentrations were proven to be significantly (14-fold) higher than those of salbutamol. Concentrations of both analytes were higher in plasma than in serum. The application of a 10-fold higher clenbuterol and salbutamol dose (2.5 mg/kg) resulted in concentrations 3- to 4-fold higher for clenbuterol and 2- to 3-fold higher for salbutamol, indicating a different release rate of these two β-agonists.
  Journal of analytical toxicology 03/2013;
• Article: EtG/EtS in Urine from Sexual Assault Victims Determined by UPLC-MS-MS.

  Solfrid Hegstad, Arne Helland, Cecilie Hagemann, Lisbeth Michelsen, Olav Spigset
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  ABSTRACT: In cases of sexual assault, victims often present too late for the detection of ethanol in biological samples. An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) method was developed and validated for the determination of ethyl glucuronide (EtG) and ethyl sulfate (EtS) in urine. Sample preparation prior to UPLC-MS-MS analysis was a simple sample dilution. The calibration ranges were 0.2-20 mg/L, and between-assay relative standard deviations were in the range of 0.7-7.0% at concentrations of 0.3, 3.0 and 7.0 mg/L. Urine samples were analyzed from 59 female patients presenting to the Sexual Assault Centre at St. Olav University Hospital in Trondheim, Norway between November 2010 and October 2011. EtG and EtS results were fully concordant, and positive in 45 of the 48 cases with self-reported alcohol intake. In contrast, ethanol was detectable in only 20 of these cases, corresponding to sensitivities of 94 and 42%, respectively. Of the patients reporting no alcohol intake, none had positive EtG/EtS findings. These data show that analysis of EtG and EtS greatly increases the detection window of alcohol ingestion in cases of sexual assault, and may shed additional light on the involvement of ethanol in such cases. The victims' self-reported intake of alcohol seems to be reliable in this study, according to the EtG/EtS findings.
  Journal of analytical toxicology 03/2013;