Arkansas City, AR, United States
Arkansas City, AR, United States

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Pulla S.,University of Arkansas for Medical Sciences | Rusch N.J.,University of Arkansas for Medical Sciences | Moran C.L.,Arkansas State Crime Laboratory | Fantegrossi W.E.,University of Arkansas for Medical Sciences | And 6 more authors.
Analytical Chemistry | Year: 2014

Opioid abuse involving emerging opioid compounds is a growing public health problem, which was highlighted recently by cases of human morbidity and mortality linked to acetyl fentanyl abuse. Unfortunately, the lack of information available on the toxicology and metabolism of acetyl fentanyl precludes its detection in human samples. The following study was conducted to test a new analytical procedure for the simultaneous quantification of acetyl fentanyl and its predicted metabolite, acetyl norfentanyl, in human urine. Metabolic reference standards and deuterium-labeled internal standards were synthesized for use in an assay that coupled solid-phase extraction (SPE) with liquid chromatography-tandem mass spectrometry (LC-MS/MS). The accuracy (% Relative Error <5%) and inter- and intrarun precision (%CV <20%) of this new method resulted in low levels of quantification (∼1 ng/mL). Similar results were obtained using liquid chromatography columns manufactured with phenyl-hexyl and biphenyl stationary phases (r2 > 0.98). Preliminary human liver microsomal and in vivo rodent studies demonstrated that acetyl fentanyl is metabolized by cytochrome P450s to acetyl norfentanyl. Urine samples from rats treated with a toxic dose of acetyl fentanyl contained high concentrations of acetyl fentanyl and acetyl norfentanyl. Further toxicokinetic studies are required to fully elucidate the metabolic pathways responsible for acetyl fentanyl detoxification and excretion. © 2013 American Chemical Society.


Moran C.L.,Arkansas State Crime Laboratory | Chimalakonda K.C.,University of Arkansas for Medical Sciences | Smedley A.L.,Arkansas State Crime Laboratory | Lackey F.D.,Arkansas State Crime Laboratory | And 13 more authors.
Analytical Chemistry | Year: 2011

"K2/SPICE" products are commonly laced with aminoalkylindole synthetic cannabinoids (i.e., JWH-018 and JWH-073) and are touted as "legal" marijuana substitutes. Here we validate a liquid chromatography- tandem mass spectrometry (LC-MS/MS) method for measuring urinary concentrations of JWH-018, JWH-073, and several potential metabolites of each. The analytical procedure has high capacity for sample throughput and does not require solid phase or liquid extraction. Evaluation of human urine specimens collected after the subjects reportedly administered JWH-018 or a mixture of JWH-018 and JWH-073 provides preliminary evidence of clinical utility. Two subjects that consumed JWH-018 primarily excreted glucuronidated conjugates of 5-(3-(1-naphthoyl)-1H-indol-1-yl)-pentanoic acid (>30 ng/mL) and (1-(5-hydroxypentyl)-1H-indol-3-yl)(naphthalene-1-yl)-methanone (>50 ng/mL). Interestingly, oxidized metabolites of both JWH-018 and JWH-073 were detected in these specimens, suggesting either metabolic demethylation of JWH-018 to JWH-073 or a nonreported, previous JWH-073 exposure. Metabolic profiles generated from a subject who consumed a mixture of JWH-018 and JWH-073 were similar to profiles generated from subjects who presumably consumed JWH-018 exclusively. Oxidized metabolites of JWH-018 and JWH-073 were of the same pattern, but JWH-018 metabolites were excreted at lower concentrations. These results begin clinically validating the LC-MS/MS assay for detecting and quantifying aminoalkylindole metabolites. Full validation awaits further testing. © 2011 American Chemical Society.


Chimalakonda K.C.,University of Arkansas for Medical Sciences | Moran C.L.,Arkansas State Crime Laboratory | Kennedy P.D.,Cayman Chemical Co. | Endres G.W.,Cayman Chemical Co. | And 9 more authors.
Analytical Chemistry | Year: 2011

The aminoalkylindole agonists JWH-018 and JWH-073 are contained in "K2/SPICE" products sold as "legal marijuana". Previous human metabolic studies have identified (ω)-hydroxyl and (ω)-carboxyl metabolites as biomarkers that are indicative of product use. However, other primary metabolites exhibiting similar chromatographic properties and mass spectra are also excreted in human urine. Analytical standards were used in this study to identify new primary metabolites as (ω-1)-hydroxyl derivatives of JWH-018 and JWH-073. The liquid chromatography tandem mass spectrometry (LC-MS/MS) procedure, coupled with an automated solid-phase extraction procedure incorporating deuterium-labeled internal standards, provides rapid resolution of the (ω)- and (ω-1) metabolites with adequate sensitivity, precision, and accuracy for trace analysis in human urine. Results from four urine specimens collected after individuals reportedly self-administered either JWH-018 or a mixture of JWH-018 and JWH-073 showed the following: (1) all tested metabolites were excreted in high concentrations, (2) (ω)- and (ω-1)-hydroxyl metabolites were exclusively excreted as glucuronic acid conjugates, and (3) ∼5%-80% of the (ω)-carboxyl metabolites was excreted as glucuronic acid conjugates. This is the first report to identify and quantify (ω-1)-hydroxyl metabolites of JWH-018 and JWH-073 and the first to incorporate automated extraction procedures using deuterium-labeled internal standards. Full clinical validation awaits further testing. © 2011 American Chemical Society.


Moran C.L.,Arkansas State Crime Laboratory | Womack M.L.,Arkansas State Crime Laboratory | Prather P.L.,University of Arkansas for Medical Sciences | Fantegrossi W.E.,University of Arkansas for Medical Sciences | And 7 more authors.
Forensic Science International | Year: 2013

New designer drugs such as K2, Spice, and "bath salts" present a formidable challenge for law enforcement and public health officials. The following report summarizes a three-year study of 1320 law enforcement cases involving over 3000 products described as vegetable material, powders, capsules, tablets, blotter paper, or drug paraphernalia. All items were seized in Arkansas from January 2010 through December 2012 and submitted to the Arkansas State Crime Laboratory for analysis. The geographical distribution of these seizures co-localized in areas with higher population, colleges, and universities. Validated forensic testing procedures confirmed the presence of 26 synthetic cannabinoids, 12 designer stimulants, and 5 hallucinogenic-like drugs regulated by the Synthetic Drug Prevention Act of 2012 and other state statutes. Analysis of paraphernalia suggests that these drugs are commonly used concomitantly with other drugs of abuse including marijuana, MDMA, and methamphetamine. Exact designer drug compositions were unpredictable and often formulated with multiple agents, but overall, the synthetic cannabinoids were significantly more prevalent than all the other designer drugs detected. The synthetic cannabinoids JWH-018, AM2201, JWH-122, JWH-210, and XLR11 were most commonly detected in green vegetable material and powder products. The designer stimulants methylenedioxypyrovalerone (MDPV), 3,4-methylenedioxy- N-methylcathinone (methylone), and α-methylamino-valerophenone (pentedrone) were commonly detected in tablets, capsules, and powders. Hallucinogenic drugs were rarely detected, but generally found on blotter paper products. Emerging designer drug products remain a significant problem and continued surveillance is needed to protect public health. © 2013 Elsevier Ireland Ltd.


Moreno L.I.,Nuclear DNA Unit | Moreno L.I.,FBI Academy | Tate C.M.,FBI Academy | Knott E.L.,Arkansas State Crime Laboratory | And 6 more authors.
Journal of Forensic Sciences | Year: 2012

The potential application of mRNA for the identification of biological fluids using molecular techniques has been a recent development in forensic serology. Constitutively expressed housekeeping genes can assess the amount of mRNA recovered from a sample, establish its suitability for downstream applications, and provide a reference point to corroborate the identity of the fluid. qPCR was utilized to compare the expression levels of housekeeping genes from forensic-like body fluid stains to establish the most appropriate assessment of human mRNA quantity prior to profiling. Although variability was observed between fluids and individuals, results indicated that beta-2 microglobulin exhibited the highest expression for all body fluids examined and across donors. A one-way analysis of variance was performed for housekeeping gene variability between donors (at the α, 0.05, significance level), and the results indicated significant differences for semen, vaginal secretions, and menstrual blood. 2012 American Academy of Forensic Sciences. Published 2012. This article is a U.S. Government work and is in the public domain in the U.S.A.


Oostdik K.,Promega Corporation | Lenz K.,Promega Corporation | Nye J.,Michigan State Police | Schelling K.,Michigan State Police | And 26 more authors.
Forensic Science International: Genetics | Year: 2014

The original CODIS database based on 13 core STR loci has been overwhelmingly successful for matching suspects with evidence. Yet there remain situations that argue for inclusion of more loci and increased discrimination. The PowerPlex® Fusion System allows simultaneous amplification of the following loci: Amelogenin, D3S1358, D1S1656, D2S441, D10S1248, D13S317, Penta E, D16S539, D18S51, D2S1338, CSF1PO, Penta D, TH01, vWA, D21S11, D7S820, D5S818, TPOX, DYS391, D8S1179, D12S391, D19S433, FGA, and D22S1045. The comprehensive list of loci amplified by the system generates a profile compatible with databases based on either the expanded CODIS or European Standard Set (ESS) requirements. Developmental validation testing followed SWGDAM guidelines and demonstrated the quality and robustness of the PowerPlex® Fusion System across a number of variables. Consistent and high-quality results were compiled using data from 12 separate forensic and research laboratories. The results verify that the PowerPlex® Fusion System is a robust and reliable STR-typing multiplex suitable for human identification. © 2014 The Authors.


Patton A.L.,Public Health Laboratory | Chimalakonda K.C.,University of Arkansas for Medical Sciences | Moran C.L.,Arkansas State Crime Laboratory | Mccain K.R.,University of Arkansas for Medical Sciences | And 5 more authors.
Journal of Forensic Sciences | Year: 2013

Limited forensic and clinical experience and the lack of confirmatory testing strategies for synthetic cannabinoids (SC) prevent adequate characterization of SC toxicity and the potential impact on public health. A statewide surveillance system identified a fatality involving a 23-year-old man found with a large stab wound to the neck following use of a SC product suspected of containing AM2201. Analytical testing for common SCs, SC metabolites, routine drugs of abuse, and over-the-counter medications was performed on heart blood obtained at autopsy. Additionally, assays were performed on the SC raw material and drug paraphernalia found on the decedent. High concentrations of AM2201 were detected in all samples. AM2201 metabolites were detected in postmortem blood. Other than a trace amount of JWH-073 found in smoke residue, no other substances were detected. Psychiatric complications including self-induced, lethal trauma can occur after the use of SC products. © 2013 American Academy of Forensic Sciences.


Chimalakonda K.C.,University of Arkansas for Medical Sciences | Hailey C.,Arkansas State Crime Laboratory | Black R.,Arkansas State Crime Laboratory | Beekman A.,Arkansas State Crime Laboratory | And 5 more authors.
Analytical Methods | Year: 2010

A new analytical method was developed and validated for the rapid determination of phencyclidine (PCP) in human blood and serum. Rapid chromatographic separation decreased the analysis time relative to standard gas chromatography (GC)-based methodologies. The method involved the use of solid-phase extraction for sample preparation and cleanup followed by liquid chromatography tandem spectrometric (LC-MS/MS) analysis and an electrospray-ionization (ESI) interface. PCP was quantified using multiple-reaction-monitoring with deuterium labeled PCP (PCP-d 5) as an internal standard. The method was validated for accuracy, precision, linearity, and recovery. The method was accurate with error <14% and precision with coefficient of variation (CV) <5.0%. The assay was linear over the entire range of calibration standards (r 2 > 0.997). The recovery of PCP after solid-phase extraction was greater than 90% with the lower limit of detection (LLOD) for PCP in 500 l of human serum after solid-phase extraction at 0.06 ng ml -1. This method was used to determine the levels of PCP in postmortem human blood samples. The LLOD in blood was 1 ng ml -1. Blood PCP concentrations were also determined separately using GC and flame ionization detection (FID). Blood calibration standards and serum calibration standards yielded similar concentrations when used to quantitate authentic human blood samples that tested positive for PCP under the GC-FID method. Extraction of PCP from serum required fewer steps and therefore could be used as a calibration matrix in place of blood. The LC-MS/MS methodology shown here was higher throughput compared with GC-based methods because of very short chromatographic run times. This was accomplished without sacrificing analytical sensitivity. © 2010 The Royal Society of Chemistry.

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