RESUMO
Methamphetamine (MA) is one of the most virulent illicit drugs that can be synthesized from household materials leading to its prevalent trafficking and local manufacturing in clandestine drug laboratories (clan labs). The significant problems of tracing MA in clan labs and monitoring drug abusers lie in the lag time between sample collection and analysis and the number of tests done. Capillary electrophoresis (CE) is a rapid separation technique amenable to miniaturization and field testing. Herein, we developed a simple transient isotachophoretic (tITP)-CE method to detect MA and its precursor pseudoephedrine (PSE) in clan labs and non-invasive biological fluids. The method was implemented on the ETD-100, a commercial fully automated portable CE instrument with an integrated swab-based extraction system. Within 2 min of insertion of the swab, MA and PSE were automatically extracted with a leading electrolyte (LE) and then separated on covalently modified capillaries. The ETD-100 showed a limit of detection (LOD) and quantification (LOQ) of MA 0.02 and 0.05 µg/swab and 0.02 and 0.06 µg/swab of PSE, with an enhancement factor of 118 and 328, respectively, when compared to a normal non-tITP injection. The intra and inter-day relative standard deviation in terms of migration time were in the range of 0.75-1.93 % for both MA and PSE and were 2.0-2.4 % for both MA and PSE peak height. The method was demonstrated with the detection of spiked MA and PSE on different household materials as well as in non-invasive biological fluids with a recovery above 60 %.
Assuntos
Eletroforese Capilar , Metanfetamina , Metanfetamina/análise , Metanfetamina/isolamento & purificação , Eletroforese Capilar/métodos , Humanos , Limite de Detecção , Pseudoefedrina/análise , Pseudoefedrina/isolamento & purificação , Detecção do Abuso de Substâncias/métodos , Detecção do Abuso de Substâncias/instrumentação , Drogas Ilícitas/análise , Drogas Ilícitas/isolamento & purificaçãoRESUMO
All pharmaceutical manufacturers are required to verify that their production equipment is free from contaminants. Here, we report the capability of a fully automated portable capillary electrophoresis instrument with an integrated sample swab extraction - the Grey Scan ETD-100 - for the detection of pharmaceutical residues on surfaces of manufacturing equipment. Lidocaine was used as a model compound and could be recovered from a surface by swabbing, extracted from the swab, and analysed within 1 min. The recovery of lidocaine from a stainless-steel coupon was 81.3 %, with a LOD of 0.13 µg/swab. This fast, sensitive, and simple method implemented on a user-friendly portable CE instrument without the need for manual sample pre-treatment provides the possibility for on-site rapid determination of equipment cleanliness in the pharmaceutical industry.
Assuntos
Indústria Farmacêutica , Aço Inoxidável , Aço Inoxidável/análise , Eletroforese Capilar , Preparações FarmacêuticasRESUMO
A procedure is described for the determination of the distribution of the contamination of banknotes with controlled drugs using tandem mass spectrometry. The method is illustrated using diacetylmorphine, which is the major active component of heroin. A series of banknotes is introduced into the mass spectrometer and the intensities of two product ions (m/z 328 and 268) derived from the precursor protonated molecule (m/z 370) are recorded. A banknote is considered contaminated if it shows a significant peak for both product ions, and if the ratio of intensities of these two peaks falls within accepted limits. The distribution of diacetylmorphine on sterling banknotes taken from general circulation within the UK can be modelled by an arcsin (square root) transformation of the data or by a log transformation of the data with a higher proportion of contamination. The two models were found to be in close agreement, predicting an upper limit (at 99.9% confidence) of contamination on banknotes from general circulation between 9 and 10%. The percentage contamination in a case study was calculated and compared to the background distribution using the two models proposed. This comparison revealed that the contamination present in the case study was inconsistent with that present on banknotes in general circulation.