Evaluation of Suspected Counterfeit Pharmaceutical Tablets Declared to Contain Controlled Substances Using Handheld Raman Spectrometers

This study describes the performance of handheld Raman devices for determining whether suspect pharmaceutical tablets declared to contain controlled substances were consistent with authentic (CWA) or not consistent with authentic (NCWA) tablets using a simple, rapid, field-friendly method capable of being used by nonexperts. Twenty-five authentic products and 84 known NCWA tablets were examined using three “parent” devices for a total of 327 analyses. On average, the parent devices yielded a true pass rate of 100%, a true fail rate of 98.4%, a false pass rate of 1.6%, and a false fail rate of 0%. The methods/libraries were then transferred to 13 identical “daughter” devices, which were used to examine 10 suspect finished dosage forms in duplicate (six known NCWA tablets and four authentic tablets) for a total of 260 measurements. On average, the daughter devices had a true pass rate of 100%, a true fail rate of 95.5%, a false pass rate of 4.5%, and a false fail rate of 0.0%. These data demonstrate that the parent–daughter electronic transfer method was successful, which permits the ability to develop methods in the laboratory that can be seamlessly pushed out to field devices. The methods can then be used to (i) prioritize samples for additional testing using other more time-consuming laboratory-based techniques needed to detect and quantify active ingredients and (ii) help support the interdiction of dangerous tablets at ports of entry, thereby preventing them from reaching the supply chain.     

Naturschutzrechtliche Vorgaben zur Verwendung gebietseigener Gehölze

Zusammenfassung  Die genetische Vielfalt ist oft übersehenes Schutzgut des Naturschutzrechts. Sie ist der Grund, warum zunehmend gefordert wird, Anpflanzungen nur mit gebietseigenem Pflanzmaterial durchzuführen. Rechtliche Probleme stellen sich hier an der Schnittstelle von Naturschutz- und Vergaberecht. Soll n?mlich bei der ?ffentlichen Auftragsvergabe zur Anpflanzung von Geh?lzen oder beim Einkauf von Pflanzmaterial nicht gegen vergaberechtliche Vorschriften versto?en werden, bedarf es hinreichender, im Naturschutzrecht verwurzelter Gründe, um ?ffentliche Ausschreibungen ausschlie?lich auf gebietseigenes Pflanzmaterial einzuengen. Diesen naturschutzrechtlichen Verpflichtungen geht der vorliegende Beitrag nach.     

GHB free acid: I. Solution formation studies and spectroscopic characterization by 1HNMR and FT-IR

In forensic evidence, gamma-hydroxybutyric acid (GHB) has frequently been encountered in one of its salt forms (gamma-hydroxybutyrate), but has also been encountered in its free acid form (GHB). Owing to the physical properties, encounters of the free acid have been largely restricted to forensic exhibits comprising aqueous solutions, such as acidic beverages that have been "spiked" or formulated with GHB salts or gamma-butyrolactone (GBL). The analysis of GHB free acid presents particular difficulties including the potential for altering the original proportions of GHB free acid, GHB carboxylate, and GBL in the course of analysis, and discrimination between GHB free acid and carboxylate forms. In this work, the formation of GHB free acid in aqueous solutions (water and/or D2O) was studied as a function of solution pH. Proton nuclear magnetic resonance (1HNMR) and Fourier-transform infrared spectrometry (FT-IR) measurements were obtained on freshly prepared mixtures of NaGHB and HCl stock solutions representing a series of points along the GHB titration curve. Both 1HNMR and FT-IR were shown to track the changing proportions of GHB free acid and carboxylate forms as a function of pH, while simultaneously monitoring for the formation of the lactone (GBL). The results were consistent with acid-base conversion behavior for a carboxylic acid. 1HNMR was shown to provide an ideal means for analysis of aqueous-based GHB/GBL forensic exhibits based on simple dilution of the neat liquid exhibit, without altering the original proportions of GHB free acid, carboxylate, and GBL in the samples.     

Identification of Opioids and Related Substances using Handheld Raman Spectrometers

This study describes the performance of handheld Raman devices for detecting one hundred opioids and related substances including fentanyl and several analogs. Using a single “parent” device, signatures (spectra) with excellent signal-to-noise ratios were generated using <5 mg of most compounds. The signatures were added to a method (library), which was electronically transferred to three “daughter” devices. The devices were able to discriminate different salt forms and isomers. On average, the daughter devices yielded a true-positive rate of 97.3% for generating an alarm for opioids and were 93.3% effective for correctly identifying the opioid. The devices yielded true-negative, false-positive and false-negative rates of 100%, 0%, and 2.7%, respectively, where false negatives were due to weak signal and fluorescence. These data demonstrate that the parent-daughter electronic transfer method was successful and effective, which permits the ability to develop methods in the laboratory that can be seamlessly pushed out to field devices.     

GHB free acid: II. Isolation and spectroscopic characterization for forensic analysis

A reference standard for gamma-hydroxybutyric acid (GHB) free acid is not commercially available, making its analysis in forensic exhibits more difficult. GHB free acid is typically encountered in aqueous solution and in the presence of the lactone, gamma-butyrolactone (GBL), presenting difficulty in Fourier transform infrared (FT-IR) analysis. The strong infrared (IR) absorptivity of the GBL carbonyl band, the shifting of the GBL carbonyl band in aqueous solutions, and the position of the O-H bend for water can mask the main carbonyl band for GHB free acid. Model solutions of beta-hydroxybutyric acid (BHB) and GBL were studied in order to further understand the masking of the GHB free acid carbonyl band in FT-IR analysis. The use of second derivative FT-IR spectroscopy was shown to provide resolution of the free acid carbonyl band, and a presumptive test for GHB free acid was developed and applied. An extension of this work included preparing, for use as a standard reference material, small amounts (< or = 10 mg) of GHB free acid. Preparation was based on the instantaneous reaction of GHB's sodium salt with a stoichiometric amount of hydrochloric acid in aqueous solution, and subsequent isolation of the free acid in neat liquid form. Both FT-IR and proton nuclear magnetic resonance spectra of the neat reference material were obtained and used to verify its identity. The isolation of GHB free acid from actual forensic exhibits is also presented, with identity confirmation using FT-IR.     

Simultaneous separation of different types of amphetamine and piperazine designer drugs by capillary electrophoresis with a chiral selector

The recent emergence of a new class of piperazine-type compounds has brought about the need for laboratory screening methods for both seized drugs and toxicological samples. These piperazine compounds, which include 1-benzylpiperazine (BZP) and 1-(3-trifluoromethylphenyl)piperazine (TFMPP), exhibit comparable physiological effects and can be substituted for the classic amphetamine-type drugs. We have optimized a chiral capillary electrophoresis (CE) separation that detects a set of 6 piperazine and 4 chiral amphetamine compounds in under 23 min using a 200 mM phosphate buffer at a pH = 2.8 with 20 mM hydroxypropyl- beta-cyclodextrin (HPbeta3CD). In addition to the above compounds, a series of "clandestine" BZP diHCl samples were also analyzed using this method to assess the ruggedness of the procedure. The novel CE separation was tailored to simultaneously detect these piperzine compounds in addition to amphetamine-type drugs. Distinct migration time and UV-spectral data were obtained for all compounds of interest.     

Der Biodiversitätsschaden nach 21a des Bundesnaturschutzgesetzes

Zusammenfassung Im Mai 2007 wurde das Gesetzes zur Umsetzung der Richtlinie des Europ?ischen Parlaments und des Rates über die Umwelthaftung zur Vermeidung und Sanierung von Umweltsch?den verabschiedet, das seinerseits die Umwelt-Haftungsrichtlinie (UH-RL) in deutsches Recht umsetzt. Auf Grund von Art. 72 Abs. 3 S. 2 GG treten Gesetze auf dem Gebiet des Naturschutzes mit Ausnahme der abweichungsfesten Teile frühestens 6 Monate nach Verkündung in Kraft. Folglich sieht Art. 4 des Gesetzes vom 10. Mai 2007 vor, dass das Umweltschadensgesetz (USchadG) und die ?nderungen im Wasserhaushaltsgesetz und im Bundesnaturschutzgesetz zum 14. November 2007 in Kraft getreten sind.     

Die kleine Novelle zur Anpassung des BNatSchG an das europäische Recht

Zusammenfassung Durch Urteil vom 10. Januar 2006 hat der Europ?ische Gerichtshof die Umsetzung der Vogelschutz-Richtlinie (V-RL) und der FFH-Richtlinie (FFH-RL) beanstandet, insbesondere der Projektbegriff der FFH-Vertr?glichkeitsprüfung sowie bestimmte Freistellungen von den artenschutzrechtlichen Verboten wurden als europarechtswidrig verworfen. Die Korrektur dieser M?ngel ist durch die sog. kleine Novelle des Bundesnaturschutzgesetzes erfolgt. Nachfolgend werden die ?nderungen des Artenschutzrechts sowie die Auswirkungen der Aufhebung des Projektbegriffs vorgestellt.     

Obama’s Human Rights Policy: Déjà vu with a Twist

In US history, much human rights policy developed in four waves during the twentieth century. These waves were triggered by similar circumstances, but all proved short-lived as structural constraints such as limited US power over other countries’ domestic actions, competing US policy priorities, a US hesitance to join multilateral institutions, and the continued domestic political weakness of human rights advocates led to setbacks. As Barack Obama took office, his campaign comments and the past patterns led to widespread expectations that he would introduce new human rights initiatives. His policies, though, would continue to face the structural constraints and would be affected by the Bush administration’s legacy. It was predictable that many of Obama’s initiatives would be only partially implemented and only partially successful. As expected, Obama’s first years have seen mixed results, but the Obama administration has advanced US human rights policies sufficiently in half-dozen key areas to say that a fifth wave of human rights policy development is underway.