Injector port acylation of γ-hydroxybutyrate (GHB): Condition optimisation, source adjustments, and characterisation of the derivatives.

For several years, gas chromatography-mass spectrometry (GC-MS) has been used to identify gamma-hydroxybutyrate (GHB) in forensic toxicology cases. However, under injector port conditions GHB can dehydrate into gamma-butyrolactone (GBL). Therefore, it is important for GHB to undergo a derivatisation reaction before an analysis to avoid the production of GBL; various analytical methods have been developed for the analysis of GHB but very few methods use acylation as a form of derivatisation.

Challenges in the identification of new thermolabile psychoactive substances: The 25I-NBOH case.

The continuous emergence of NPS over the last years poses a series of novel challenges for forensic analysts. Most of those new compounds are synthesized with minimal chemical modifications to the structure of already known chemicals in order to avoid regulations. Some of these new compounds may undergo chemical changes during analysis leading to misidentification and detrimental legal consequences.

Classification of ANFO samples based on their fuel composition by GC-MS and FTIR combined with chemometrics.

Ammonium nitrate fuel oil (ANFO) is one of the most favorite explosives used in terrorist attacks. This explosive is a complex mixture of 95-96% ammonium nitrate (AN) and 4-5% liquid hydrocarbons (fuel oil). In this study, we analyze a variety of ANFO explosive mixtures in order to classify their different sources of origin by observing the difference in fuel components.

Keeping pace with NPS releases: fast GC-MS screening of legal high products.

The continuous appearance of novel psychoactive substances (NPS) in legal high products presents a challenge for the routine analytical laboratory. A rapid screening method for NPS analysis using fast gas chromatography mass spectrometry (fast GC-MS) is presented. Twenty-three analytes, including 5-iodo-2-aminoindane (5-IAI), 1-(thiophen-2-yl)-2-methylaminopropane (MPA), 1-benzylpiperazine (BZP), 4-methylmethcathinone (mephedrone), 5,6-methylenedioxy-2-aminoindane (MDAI) and methoxetamine (MXE) were separated within 4 min.

Investigation into the suitability of capillary tubes for microcrystalline testing.

A comparison between microcrystalline tests performed on microscope slides and flat capillary tubes with inner diameters ranging from 0.1 to 0.7 mm was carried out to explore the appropriateness of tubes for rapid testing of suspected drugs of abuse in the laboratory as well as in the field.

Injection port silylation of γ-hydroxybutyrate and trans-hydroxycrotonic acid: conditions optimisation and characterisation of the di-tert-butyldimethylsilyl derivatives by GC-MS.

Silylation is usually carried out on γ-hydroxybutyrate (GHB) for its analysis by Gas Chromatography/Mass Spectrometry (GCMS) and requires potentially long incubation times before injection during which the derivatisation reagent and derivatives (such as trimethyl-silyl compounds) can hydrolyse. Moreover, alternative internal standards (IS) are often useful depending on sample matrices, extraction/purification procedures, commercial availability and price. This study evaluated the possibility of silylating GHB with an injection port derivatisation procedure using N-methyl-N-[tert-butyldimethyl-silyl]trifluoroacetimide (MTBSTFA) with 1% tert-butyldimethylchlorosilane (TBCS) as the derivatisation reagent, producing di-tert-butyldimethyl-silyl derivatives as a novel means of analyzing GHB.

Microcrystalline identification of selected designer drugs.

A microcrystalline test for the detection of 4-methylmethcathinone (mephedrone), benzylpiperazine (BZP) and 5,6-methylenedioxy-2-aminoindane (MDAI) using aqueous solutions of mercury chloride is described. Each of the compounds investigated formed specific drug-reagent crystals within minutes. The uniqueness of the test was confirmed by comparison of the microcrystalline response to that of other psychoactive stimulants and a common cutting agent.

An analysis of legal highs: do they contain what it says on the tin?

In recent years the availability of so-called legal highs over the Internet has hugely increased. Numerous online legal-high retailers market a broad variety of products which are advertised as research chemicals, bath salts, or plant food although clearly intended for human consumption as recreational drug replacements. No guidelines exist as to what is sold and in what purity.

Reversing microcrystalline tests--an analytical approach to recycling of microcrystals from drugs of abuse.

A combined analysis of microcrystalline tests followed by LC-MS or GC-MS analysis is described. Microcrystalline tests are shown to be non-destructive as addition products formed were easily dissociated after the application of an appropriate solvent. Subsequent analysis of the sample was done to quantify the recovery of the drug.

Enhancement of microcrystalline identification of gamma-hydroxybutyrate.

An enhancement of the microcrystalline test for the detection of gamma-hydroxybutyrate (GHB) is described. The original test used a silver/copper reagent which consisted of 0.1 g of silver nitrate and 0.