Special Testing and Research Laboratory

Dulles Town Center, VA, United States

Special Testing and Research Laboratory

Dulles Town Center, VA, United States
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Casale J.F.,Special Testing and Research Laboratory | Mallette J.R.,Special Testing and Research Laboratory | Guest E.M.,Special Testing and Research Laboratory
Forensic Chemistry | Year: 2017

The United States is currently in the midst of an unprecedented illicit fentanyl crisis. In the last year alone there have been more recent fentanyl-related overdose deaths than in the previous 60 years. The current crisis is multi-faceted and involves a global supply of fentanyl and related substances being smuggled into the United States. Illicit carfentanil hydrochloride has recently entered the drug market causing multiple overdoses and deaths across the U.S. To date, over 400 confirmed carfentanil cases have been identified. Carfentanil is approximately 100 times more potent that fentanyl with only 20 μg of material required to produce a lethal dose. Due to a lack of published spectra for carfentanil HCl, analytical profiles are provided for three recent carfentanil submissions to our laboratory which include infrared spectroscopy, nuclear magnetic resonance spectroscopy, gas chromatography-mass spectrometry, isotope ratio mass spectrometry, and quantitative determination via gas chromatography–flame ionization detection. The three submissions were determined to contain 0.62%, 1.87%, and 0.31% carfentanil HCl, respectively. Each exhibit also contained a fentanyl-related substance (fentanyl or 2-furanylfentanyl). Acetylcarfentanil was characterized as an impurity in two exhibits. Isotopic analyses of two exhibits suggest they are intimately related. © 2017

News Article | February 16, 2017
Site: news.yahoo.com

In this photo released by the US Drug Enforcement Agency, DEA, and taken on Oct. 21, 2016, a sample of carfentanil is being analyzed at the DEA’s Special Testing and Research Laboratory in Sterling, Va. China is adding the deadly elephant tranquilizer carfentanil and three related synthetic opioids to its list of controlled substances effective March 1, China's National Narcotics Control Commission said Thursday. (Russell Baer/U.S. Drug Enforcement Administration via AP) SHANGHAI (AP) — So deadly it's considered a terrorist threat, carfentanil has been legal in China— until now. Beijing is banning carfentanil and three similar drugs as of March 1, China's Ministry of Public Security said Thursday, closing a major regulatory loophole in the fight to end America's opioid epidemic. "It shows China's attitude as a responsible big country," Yu Haibin, the director of the Office of the National Narcotics Control Committee, told the Associated Press. "It will be a strong deterrent." He added that China is actively considering other substances for sanction, including U-47700, an opioid marketed as an alternative to banned fentanyls. China said the March 1 ban will also apply to carfentanil's less-potent cousins furanyl fentanyl, acryl fentanyl and valeryl fentanyl. The U.S. Drug Enforcement Administration called China's move a potential "game-changer" that is likely to have a big impact in the U.S., where opioid demand has driven the proliferation of a new class of deadly drugs made by nimble chemists to stay one step ahead of new rules like this one. After China controlled 116 synthetic drugs in October 2015, seizures in the United States of compounds on that list plunged. "It's a substantial step in the fight against opioids here in the United States," said Russell Baer, a DEA special agent in Washington. "We're persuaded it will have a definite impact." Legally used as an anesthetic for elephants and other large animals, carfentanil burst into the North American drug supply last summer, causing hundreds of unsuspecting drug users to overdose. The DEA confirmed more than 400 seizures of carfentanil across eight U.S. states from July through October. So lethal an amount smaller than a poppy seed can kill a person, carfentanil was researched for years as a chemical weapon and used by Russian forces to subdue Chechen separatists at a Moscow theater in 2002. New data from DEA laboratories suggests the supply of furanyl fentanyl is now surging. DEA labs identified 44 samples of furanyl fentanyl in the last three months of 2016, up three-fold from the prior quarter. Though Beijing has said U.S. assertions that China is the top source of fentanyls lack evidence, the two countries have deepened cooperation as the U.S. opioid epidemic intensifies. Beijing already regulates fentanyl and 18 related compounds, even though they are not widely abused domestically. Since 2016, China has arrested dozens of synthetic drug exporters, destroyed eight illegal labs and seized around 2 tons of new psychoactive substances, according to the Office of the National Narcotics Control Committee. But the battle against rapidly evolving synthetic drugs is complicated by the deeply global nature of the narcotics trade and the deeply national nature of law enforcement. Some online drug vendors host their websites on servers abroad to thwart police. All benefit by submerging their illicit packages in the vast tides of legitimate commerce shipped or sent by courier from China. One example of the kind of global coordination needed to take down synthetic drug barons is the case of Zhang Lei, whom the U.S. Treasury Department designated a drug kingpin in 2014. China shared 4,221 clues with 58 countries and areas in the hunt for Zhang, Chinese drug control authorities said Thursday. Zhang was sentenced to 14 years in Chinese prison last year, according to one of his lawyers, Fan Renzhong. In October, the AP identified 12 Chinese companies willing to export carfentanil around the world for a few thousand dollars a kilogram (2.2. pounds), no questions asked. That same month China began evaluating whether to ban carfentanil and the three other drugs. Usually, the process can take nine months. This time, it took just four. Good international cooperation and effective early warning systems to track the emergence of novel drugs helped speed the process, Chinese drug control officials said Thursday. China's action is "a hopeful sign of political and strategic law enforcement cooperation," said Jeremy Douglas, a regional representative for the U.N. Office on Drugs and Crime in Bangkok. "But having legislation is a first step. The law will need to be enforced effectively." Offers for carfentanil from Chinese vendors were scarce Thursday, but the AP quickly secured five offers to export furanyl fentanyl to the United States. Some vendors also pushed U-47700. "One news I just got is that the carfentanil and furanyl fentanyl etc opioid analogs will be controlled in China on March 1 effective," one vendor called Ete wrote in an email. "So if you need them pls make it before that day. After that day it will be unavailable." The vendor did not immediately respond to a request for comment from AP. Associated Press researcher Fu Ting contributed to this report from Shanghai.

Lurie I.S.,Special Testing and Research Laboratory | Berrier A.L.,Special Testing and Research Laboratory | Casale J.F.,Special Testing and Research Laboratory | Iio R.,Forensic Science Laboratory | Bozenko Jr. J.S.,Special Testing and Research Laboratory
Forensic Science International | Year: 2012

Methodology is presented for the profiling of fentanyl in seized drugs using ultra high performance liquid chromatography in combination with tandem mass spectrometry (UHPLC-MS/MS). Target analysis was performed for 40 fentanyl processing impurities, several of which are markers for a specific synthetic route (Siegfried or Janssen). For the separation of these solutes, an Acquity BEH C18 1.7. μm particle column (150. mm. ×. 2.1. mm) with a binary 1% formic acid (pH 2.0)/acetonitrile gradient was used. For MS/MS detection, an atmospheric pressure positive electrospray source was employed with selected reaction monitoring (SRM). The coupling of the high separation power of UHPLC with the highly selective and sensitive detection of MS/MS is amenable to the determination of synthetic route and linking of drug seizures. The technology is also applicable to exhibits containing trace levels of fentanyl in the presence of significantly excess amounts of heroin and/or adulterants. © 2012 .

Li L.,Special Testing and Research Laboratory | Lurie I.S.,George Washington University
Forensic Science International | Year: 2014

The use of psychoactive "designer drugs" has increased rapidly due to their varying and sometimes ambiguous legal status and their ready access via the Internet and at local "headshops." A quick screening method for samples containing these substances, using ultra-high performance liquid chromatography with photodiode array UV and mass spectrometric detection (UHPLC-PDA/UV-MS), is presented. The method enables the screening of a variety of samples containing emerging/reemerging drugs, including β-keto phenethylamines (cathinone derivatives), synthetic cannabinoids/cannabimimetics, and phenethylamine derivatives. The use of dual detectors not only provides molecular weight information but also differentiates the drugs by their categories and in some cases even their sub-categories. Moreover, ring positional isomers of cathinone and phenethylamine derivatives can be easily differentiated by their retention times and UV spectra. © 2014.

Li L.,Special Testing and Research Laboratory | Lurie I.S.,Special Testing and Research Laboratory | Lurie I.S.,George Washington University
Forensic Science International | Year: 2015

Designer: phenethylamines (PEAs) and cathinones have been encountered worldwide. Complete characterization of these substances can be challenging due to their chirality and variably substituted phenyl rings. In this study, 24 PEAs and cathinones were analyzed by ultra high performance liquid chromatography with photo diode array detection (UHPLC-PDA) on a variety of stationary phases, and by capillary electrophoresis on a dynamically coated capillary with PDA detection (CE-PDA). In the UHPLC-PDA study, a BEH Phenyl column resolved 18 of the 24 regioisomers in 8. min, with good discrimination of the PEAs. In contrast, capillary zone electrophoresis (CZE) on a dynamically coated capillary partially or baseline resolved only 10 of the 24 regioisomers, but with improved discrimination of mono-substituted cathinones. A second series of CE-PDA experiments using 80. mM (2-hydroxypropyl)-β-cyclodextrin (HP-β-CD) in the run buffer resolved all 24 regioisomers and all but two sets of enantiomers within 18. min. Five illicit samples were successfully analyzed using the described methods. © 2015 Published by Elsevier Ireland Ltd.

Mallette J.R.,Special Testing and Research Laboratory | Casale J.F.,Special Testing and Research Laboratory
Journal of Chromatography A | Year: 2014

The isomeric truxillines are a group of minor alkaloids present in all illicit cocaine samples. The relative amount of truxillines in cocaine is indicative of the variety of coca used for cocaine processing, and thus, is useful in source determination. Previously, the determination of isomeric truxillines in cocaine was performed with a gas chromatography/electron capture detection method. However, due to the tedious sample preparation as well as the expense and maintenance required of electron capture detectors, the protocol was converted to a gas chromatography/flame-ionization detection method. Ten truxilline isomers (alpha-, beta-, delta-, epsilon-, gamma-, omega, zeta-, peri-, neo-, and epi-) were quantified relative to a structurally related internal standard, 4',4″-dimethyl-α-truxillic acid dimethyl ester. The method was shown to have a linear response from 0.001 to 1.00. mg/mL and a lower detection limit of 0.001. mg/mL. In this method, the truxillines are directly reduced with lithium aluminum hydride and then acylated with heptafluorobutyric anhydride prior to analysis. The analysis of more than 100 cocaine hydrochloride samples is presented and compared to data obtained by the previous methodology. Authentic cocaine samples obtained from the source countries of Colombia, Bolivia, and Peru were also analyzed, and comparative data on more than 23,000 samples analyzed over the past 10 years with the previous methodology is presented. © 2014.

Lurie I.S.,Special Testing and Research Laboratory | Driscoll S.E.,Special Testing and Research Laboratory | Cathapermal S.S.,Special Testing and Research Laboratory | Panicker S.,Special Testing and Research Laboratory
Forensic Science International | Year: 2013

Rapid, precise, accurate, and reproducible methodology using ultra-high-pressure liquid chromatography (UHPLC) for the analysis of heroin and basic impurities is described. The determination of heroin, morphine, O3-monoacetylmorphine, O6-monoacetylmorphine, codeine, acetylcodeine, noscapine, and papaverine is accomplished using reversed-phase chromatography (RPC), employing a 1.7μm Acquity UPLC BEH C18 column (2.1. mm. ×. 150. mm) with a phosphate buffer (pH 1.6)-acetonitrile gradient and PDA detection. The target analytes are well resolved from each other and most adulterants in less than 20. min. For the few instances when adulterants interfere with target analytes, a 1.7μm Acquity CSH Fluoro-Phenyl (2.1. mm. ×. 150. mm) column is utilized with the same gradient conditions. The reported methodology can detect impurities as low as 0.02% relative to heroin, and is well suited for heroin profiling. © 2013.

Lurie I.S.,Special Testing and Research Laboratory | Li L.,Special Testing and Research Laboratory | Toske S.G.,Special Testing and Research Laboratory
Journal of Chromatography A | Year: 2011

The use of hydrophilic interaction chromatography (HILIC) with sub 2 μm particle columns for the analysis of drugs and related compounds of forensic interest is described. This technique uses a high organic/low aqueous buffered mobile phase with a polar stationary phase, and is excellent for the separation of many of the charged solutes that are found in forensic drug exhibits. In this study, HILIC is investigated for 11 solutes of forensic interest, including weak bases, weak acids, and a neutral solute. In addition, for columns containing either ethylene bridged hybrid particles with or without an amide bonded phase, the effects of acetonitrile concentration, buffer type, buffer concentration, linear velocity, and sample concentration were studied. Based on these studies, HILIC with sub 2 μm particle columns can offer highly efficient, selective, and rapid isocratic separations of drugs and related compounds of forensic interest, with excellent peak shapes and low back pressures. This is in contrast to reverse phase chromatography (RPLC), where gradient elution is usually required, which can result in extensive overlap between acidic, neutral, and basic solutes. In addition, since HILIC exhibits a much greater loading capacity than RPLC, it could be a preferred technique for drug profiling. Furthermore, because high organic content mobile phases are highly amenable to mass spectrometric detection, the use of HILIC with tandem mass spectrometric detection for the analysis of seized drugs is described. © 2011.

Morello D.R.,Special Testing and Research Laboratory | Cooper S.D.,Special Testing and Research Laboratory | Panicker S.,Special Testing and Research Laboratory | Casale J.F.,Special Testing and Research Laboratory
Journal of Forensic Sciences | Year: 2010

The illicit manufacture of heroin results in the formation of trace level acidic and neutral impurities. These impurities are detectable in illicit heroin and provide valuable information about the manufacturing process used. The isolation, derivatization, and semiquantitative analysis of neutral and acidic heroin manufacturing impurities by programmed temperature vaporizing injector-gas chromatography-mass spectrometry (PTV-GC-MS) is described. Trace acidic and neutral heroin impurities were isolated from basic fractions using liquid-liquid extraction. Extracted impurities were treated with N-Methyl-N-trimethylsilyltrifluoroacetamide followed by PTV-GC-MS analyses. Semiquantitative data were obtained using full scan mass spectrometry utilizing unique ions or ion combinations for 36 trace impurities found in crude and/or highly refined heroin samples. Minimum detection limits for acidic and neutral impurities were estimated to be at the 10-7 level relative to total morphine. Over 500 authentic heroin samples from South America, Mexico, Southwest Asia, and Southeast Asia were analyzed. Classification of illicit heroin based on the presence or absence and relative amounts of acidic and neutral impurities is presented. © 2007 American Academy of Forensic Sciences.

Mallette J.R.,Special Testing and Research Laboratory | Casale J.F.,Special Testing and Research Laboratory
Journal of Forensic Sciences | Year: 2015

This study presents data that establish the makeup of solvents utilized in illicit cocaine hydrochloride production, as determined via the identification of the occluded solvents in the crystal matrix of the final product. The occluded solvent ratios can differ dramatically from the ratios of the original processing solvents. Additionally, the presented data suggest the diversion of commercial solvents to illicit cocaine hydrochloride laboratories. Thirty-five commercial solvents were obtained from five chemical manufacturing companies in South America. Each solvent was qualitatively and quantitatively analyzed using static headspace-gas chromatography-mass spectrometry (HS-GC-MS). After obtaining the chemical profile for each commercial solvent, solvents and/or solvent mixtures were prepared to be comparable in composition to several of the commercial products. Over 90 individual batches of cocaine hydrochloride were prepared from cocaine base using these solvents or solvent mixtures, which match those most commonly employed in clandestine laboratories. Additionally, a number of unique manufacturing by-products produced from processing solvents were identified, and their significance is discussed. © 2014 American Academy of Forensic Sciences.

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