Di-(<i>β</i>-Phenylisopropyl)amine in Illicit Amphetamine

Huizer, Henk; Brussee, H.; Meer, A.J. Poortman-van der

doi:10.1520/jfs11822j

Cited by 21 publications

(8 citation statements)

References 9 publications

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“…This similar peak pattern was evidence, that the used SPE procedure was capable to extract the various organic compounds from the aqueous waste samples which were identified as following:Benzyl alcohol (A) is an impurity which was up to now only reported in methamphetamine samples 31,32. 4M5PP is one of the most commonly reported impurities of amphetamine12,33,35,40,41,[45][46][47] and considered route specific for the Leuckart reaction. This compound (F) was also found by others in methamphetamine31,32,[34][35][36] and in amphetamine 12,37 samples.…”

supporting

confidence: 62%

“…This is supported by the fact, that Arnoldi et al 37 analysed 'wet' amphetamine which usually contains large amounts of solvents (methanol). Phenylacetic acid is a possible pre-precursor to produce BMK, 33,42,43 12,33,35,40,41,[45][46][47] and considered route specific for the Leuckart reaction. [48][49][50][51] It is formed from the reaction of BMK with 2 formamide molecules during the first Leuckart step together with the isomer 4-benzylpyrimidine (P) which is also considered route specific.…”

Section: Solid-phase Extraction Gas Chromatographymass Spectrometrymentioning

confidence: 99%

“…N-(β-phenylisopropyl)benzyl methyl ketimine (V) was reported to be formed from the condensation between BMK and amphetamine 33,50. N,N-di-(β-phenylisopropyl)amine (W) is a very common impurity in amphetamine samples which is formed during the first Leuckart step 12,14,35,45,47,50. 1,3-dimethyl-2-phenylnapthalene (Y) was reported in methamphetamine32,36 and amphetamine14,41 studies before and is formed from BMK in an acidic environment.An unknown compound (L), which was not included in the used database, was found in sample 12GAPAAN at a high intensity.…”

mentioning

confidence: 99%

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Characterisation of aqueous waste produced during the clandestine production of amphetamine following the Leuckart route utilising solid‐phase extraction gas chromatography–mass spectrometry and capillary electrophoresis with contactless conductivity detection

Hauser

Hulshof

Rößler

et al. 2018

Drug Testing and Analysis

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Chemical waste from the clandestine production of amphetamine is of forensic and environmental importance due to its illegal nature which often leads to dumping into the environment. In this study, 27 aqueous amphetamine waste samples from controlled Leuckart reactions performed in Germany, the Netherlands, and Poland were characterised to increase knowledge about the chemical composition and physicochemical characteristics of such waste. Aqueous waste samples from different reaction steps were analysed to determine characteristic patterns which could be used for classification. Conductivity, pH, density, ionic load, and organic compounds were determined using different analytical methods. Conductivity values ranged from 1 to over 200 mS/cm, pH values from 0 to 14, and densities from 1.0 to 1.3 g/cm . A capillary electrophoresis method with contactless conductivity detection (CE-C D) was developed and validated to quantify chloride, sulphate, formate, ammonium, and sodium ions which were the most abundant ions in the investigated waste samples. A solid-phase extraction sample preparation was used prior to gas chromatography-mass spectrometry analysis to determine the organic compounds. Using the characterisation data of the known samples, it was possible to assign 16 seized clandestine waste samples from an amphetamine production to the corresponding synthesis step. The data also allowed us to draw conclusions about the synthesis procedure and used chemicals. The presented data and methods could support forensic investigations by showing the probative value of synthesis waste when investigating the illegal production of amphetamine. It can also act as starting point to develop new approaches to tackle the problem of clandestine waste dumping.

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supporting

confidence: 62%

Section: Solid-phase Extraction Gas Chromatographymass Spectrometrymentioning

confidence: 99%

mentioning

confidence: 99%

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Characterisation of aqueous waste produced during the clandestine production of amphetamine following the Leuckart route utilising solid‐phase extraction gas chromatography–mass spectrometry and capillary electrophoresis with contactless conductivity detection

Hauser

Hulshof

Rößler

et al. 2018

Drug Testing and Analysis

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“…This route is well known and several instructions are available from Internet sources and publications which were adapted for this study. 7,11,26,[29][30][31][32] First a complete 4-step Leuckart synthesis of amphetamine sulphate starting from APAAN was performed. After each synthesis step, a part of the organic phase was collected and analysed using gas chromatography-mass spectrometry (GC-MS).…”

Section: Synthesesmentioning

confidence: 99%

Identification of specific markers for amphetamine synthesised from the pre‐precursor APAAN following the Leuckart route and retrospective search for APAAN markers in profiling databases from Germany and the Netherlands

Hauser

Rößler

Hulshof

et al. 2017

Drug Testing and Analysis

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α-Phenylacetoacetonitrile (APAAN) is one of the most important pre-precursors for amphetamine production in recent years. This assumption is based on seizure data but there is little analytical data available showing how much amphetamine really originated from APAAN. In this study, several syntheses of amphetamine following the Leuckart route were performed starting from different organic compounds including APAAN. The organic phases were analysed using gas chromatography-mass spectrometry (GC-MS) to search for signals caused by possible APAAN markers. Three compounds were discovered, isolated, and based on the performed syntheses it was found that they are highly specific for the use of APAAN. Using mass spectra, high resolution MS and nuclear magnetic resonance (NMR) data the compounds were characterised and identified as 2-phenyl-2-butenenitrile, 3-amino-2-phenyl-2-butenenitrile, and 4-amino-6-methyl-5-phenylpyrimidine. To investigate their significance, they were searched in data from seized amphetamine samples to determine to what extent they were present in illicitly produced amphetamine. Data of more than 580 cases from amphetamine profiling databases in Germany and the Netherlands were used for this purpose. These databases allowed analysis of the yearly occurrence of the markers going back to 2009. The markers revealed a trend that was in agreement with seizure reports and reflected an increasing use of APAAN from 2010 on. This paper presents experimental proof that APAAN is indeed the most important pre-precursor of amphetamine in recent years. It also illustrates how important it is to look for new ways to identify current trends in drug production since such trends can change within a few years.

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“…The organic solvents were removed under reduced pressure, and the aqueous residue was extracted with 50 mL of dichloromethane. The dichloromethane solution was dried with magnesium sulphate, filtered, and removed under reduced pressure to [11] [bis(1-methyl-2-phenylethyl)formamide] 2,4-Dimethyl-3,5-diphenyl-pyridine [13,14] N-(b-Phenyl-isopropyl)benzyl methyl ketimine [15] [N-…”

Section: Synthesis Of By-productsmentioning

confidence: 99%