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A rapid, sensitive, accurate, precise, reproducible, and versatile method for determining the purity of reference drug standards and the routine analysis of illicit drugs and adulterants using proton (1H) Nuclear Magnetic Resonance (NMR) Spectroscopy is presented. The methodology uses a weighed sample dissolved in a deuterated solvent or solvent mixture(More)
A rapid, accurate, precise, reproducible, economical, and environmentally gentle method using capillary electrophoresis (CE) is presented for the routine analysis of methamphetamine, amphetamine, MDA, MDMA, MDEA, and cocaine in seized drugs. The methodology uses a 32 cm by 50 microm capillary (length to detector 23.5 cm) with a commercially available buffer(More)
In NMR, peak area quantitation is the most common method used because the area under a peak or peak group is proportional to the number of nuclei at those frequencies. Peak height quantitation has not enjoyed as much utility because of poor precision and linearity as a result of inconsistent shapes and peak widths (measured at half height). By using a(More)
A rapid, precise, accurate, and robust method using capillary electrophoresis (CE) with dynamically coated capillaries for the analysis of the major opium alkaloids in opium is presented. Dynamic coating of the capillary surface is accomplished using a commercially available reagent kit (polycation coating followed by polyanion coating). The addition of(More)
Four new impurities have recently been detected in the gas chromatographic signature profiles of many illicit cocaine hydrochloride exhibits. These impurities are only seen in exhibits that have been oxidized and are most prominent in samples that have been highly oxidized. Exhibits containing these compounds were subjected to gas and liquid(More)
Illicitly produced heroin is commonly cut with carbohydrates to increase bulk. The analysis of these solutes is important for legal and intelligence purposes. A capillary electrophoresis (CE) method was developed for the qualitative analysis of dextrose, lactose, sucrose, inositol, and mannitol in heroin exhibits. For this method, a 64 cm (55.5 cm to(More)
The analysis of by-products and impurities in illicit cocaine, including the isomeric truxillines, is important for derivation of both strategic and tactical intelligence. In the present study, various capillary electrophoresis techniques were investigated for this purpose. The use of the anionic beta-cyclodextrin sulfobutyl ether IV as a run buffer(More)
The evaluation of a fully automated quantitative proton nuclear magnetic resonance spectroscopy (qNMR) processing program, including the determination of its processing uncertainty, and the calculations of the combined uncertainty of the qNMR result, is presented with details on the use of a trimmed purity average. Quantitative NMR spectra (1359) were(More)
Desacetyldiltiazem and an uncharacterized artifactual compound with an apparent mass of 354 Daltons have been observed in gas chromatographic profiles of cocaine exhibits containing diltiazem. The use of methanol as an injection solvent for cocaine samples containing sodium bicarbonate causes the formation of these compounds in the injection port; however,(More)
A trace processing impurity found in certain methamphetamine exhibits was isolated and identified as trans-N-methyl-4-methyl-5-phenyl-4-penten-2-amine hydrochloride (1). It was determined that this impurity was produced via reductive amination of trans-4-methyl-5-phenyl-4-penten-2-one (4), which was one of a cluster of related ketones generated during the(More)