Determination of phenylethylamines in hallucinogenic cactus species by high-performance liquid chromatography with photodiode-array detection

Helmlin, H. J.; Bourquin, Daniel; Brenneisen, Rudolf

doi:10.1016/0021-9673(92)80380-d

Cited by 17 publications

(7 citation statements)

References 13 publications

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“…The chromatographic system described here was originally developed for the analysis of methadone in pharmaceutical preparations (48). Subsequently, it was routinely used in our laboratory for the analysis of psychotropic substances in biological matrix (e.g., determination of cathinone and its metabolites in plasma [49] and urine [50] as well as for MDMA and MDA in urine [35]).…”

Section: Hplc Analysismentioning

confidence: 99%

Analysis of 3,4-Methylenedioxymethamphetamine (MDMA) and its Metabolites in Plasma and Urine by HPLC-DAD and GC-MS

Helmlin

Bracher

Bourquin

et al. 1996

Journal of Analytical Toxicology

133

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In Europe, the compound 3,4-methylenedioxymethamphetamine (MDMA, Ecstasy, Adam), in addition to cannabis, is the most abused illicit drug at all-night "techno" parties. Methods for the determination of MDMA and its metabolites, 4-hydroxy-3-methoxymethamphetamine (HMMA), 3,4-dihydroxy-methamphetamine (HHMA), 3,4-methylenedioxyamphetamine (MDA), 4-hydroxy-3-methoxyamphetamine (HMA), and 3,4-dihydroxyamphetamine (HHA), in biological fluids were established. Plasma and urine samples were collected from two patients in a controlled clinical study over periods of 9 and 22 h, respectively. MDMA and MDA were determined in plasma and urine by reversed-phase high-performance liquid chromatography with diode array detection (HPLC-DAD) after solid-phase extraction on cation-exchange columns. Acidic or enzymatic hydrolysis was necessary to detect HMMA, HMA, HHMA, and HHA, which are mainly excreted as glucuronides. Gas chromatography-mass spectrometry (GC-MS) was used for confirmation. Sample extraction and on-disc derivatization with heptafluorobutyric anhydride (HFBA) were performed on Toxi-Lab SPEC solid-phase extraction concentrators. After administration of a single oral dose of 1.5 mg/kg body weight MDMA, peak plasma levels of 331 ng/ml MDMA and 15 ng/mL MDA were measured after 2 h and 6.3 h, respectively. Peak concentrations of 28.1 micrograms/mL MDMA in urine appeared after 21.5 h. Up to 2.3 micrograms/mL MDA, 35.1 micrograms/mL HMMA, and 2.1 micrograms/mL HMA were measured within 16-21.5 h. Conjugated HMMA and HHMA are the main urinary metabolites of MDMA.

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Section: Hplc Analysismentioning

confidence: 99%

Analysis of 3,4-Methylenedioxymethamphetamine (MDMA) and its Metabolites in Plasma and Urine by HPLC-DAD and GC-MS

Helmlin

Bracher

Bourquin

et al. 1996

Journal of Analytical Toxicology

133

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“…fricii and L. williamsii var. decipiens, consisted of an extended AT sequence that included one set of TTT bases within its AT-rich region: TT(AT) 4 ATTT(AT) 9 AA. Genotype 10, from two samples identified as L. williamsii var.…”

Section: Trnl/trnf Regionmentioning

confidence: 99%

“…, using sequences of the rpl16 gene to classify 62 members of Cacteae, a tribe of the Cactaceae, proposed a division of the genus Lophophora , with L. williamsii related to members of genus Obregonia and L. diffusa related to genus Acharagma . As L. williamsii contains an illegal substance with the potential to be abused and L. diffusa does not , it is imperative that forensic analysis methodologies be developed for the identification of Lophophora tissue samples. In this study, we explore DNA analysis of the noncoding DNA between the chloroplast trnL and trnF genes ( trnL / trnF region) and the chloroplast rbcL gene as a method to aid in: (i) distinguishing between members of the Lophophora genus and species outside the Lophophora genus; (ii) differentiating between species within the Lophophora genus; and (iii) identifying single individuals in the Lophophora genus.…”

mentioning

confidence: 99%

Identification and Individualization of Lophophora using DNA Analysis of the trnL/trnF Region and rbcL Gene

Ng¹,

Sandoval²,

Murphy

2015

Journal of Forensic Sciences

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Lophophora williamsii (peyote) is a small, spineless, greenish-blue cactus found in Mexico and the southwestern United States. Ingestion of the cactus can result in hallucinations due to its content of mescaline. In the United States, L. williamsii is classified as a Schedule I controlled substance. In this study, we use DNA analysis of the chloroplast trnL/trnF region and chloroplast rbcL gene to identify the individuals of Lophophora. Using the rbcL gene, Lophophora specimens could be distinguished from outgroups, but species within the genus could not be distinguished. The trnL/trnF region split the Lophophora genus into several groups based on the length and substructure of an AT-rich segment of the sequence. Our results indicate that the genetic variability at the trnL/trnF locus is greater than previously recognized. Although DNA structures at the trnL/trnF region and rbcL gene do not align with the classification of Lophophora species, they can be used to aid in forensic analysis.

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“…However, in the United States Pharmacopoeia [ 5 ] (USP), quantitation methods for methadone in pharmaceutical preparations are based on acid titration, UV determination, GC, and High Performance Liquid Chromatography (HPLC). Some of these methods present, as do HPLC methods described in the literature for methadone analysis, the following disadvantages: lenghthy and wasteful use of solvent analysis (gradient elution over 10–20 min), a tedious extraction procedure (not suited for routine analysis) or the use of a fluorescent ion-pairing agent [ 6 – 10 ].…”

Section: Introductionmentioning

confidence: 99%

Development and validation of a HPLC-UV method for methadone hydrochloride quantification in a new oral solution with preservatives to be implemented in physicochemical stability studies

et al. 2022

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Purpose The Pharmacy Service of the Infanta Leonor University Hospital acquires, compounds, distributes and dispenses more than 3000 L of methadone oral solution to Drug Addiction Patients Centers per year. Our purpose is to develop and validate an improved high performance liquid chromatography (HPLC) method to quantify methadone hydrochloride in a new oral solution with methylhydroxybenzoate (methylparaben) and propylhydroxybenzoate (propylparaben) to be implemented in physicochemical stability studies that allow to provide more information and even to increase the beyond-use date. Methods A HPLC-Agilent® 1100 equipment, comprising a quaternary pump and an ultraviolet diode-array-detector (DAD) was used. An analytical method development and validation was completed. The curve was constructed from methadone working concentrations of 75–125% (7.5, 9.0, 10.0, 11.0 and 12.5 mg/mL) to assess the linear relationship between the concentration of the analyte and the obtained areas. Precision and accuracy were calculated. Detection and quantification limit (LD, LQ) were estimated using the EURACHEM method. Forced-degradation studies were also performed. Results Chromatographic conditions were: flow rate 1.6 mL/min; mobile phase 55% acetonitrile and 45% sodium phosphate 25 mM (pH = 10); injection volume was 5 µL. The column was a Waters-XTerra™ RP18, maintained at 40 °C. DAD was λ = 254 nm. Retention times for methadone, methylparaben and propylparaben were 4.34, 0.70 and 0.88 min respectively. The method was linear (y = 284.3x − 97.8, r = 0.996). Instrumental precision was 0.33% for standards (n = 10); intra-assay precision 0.53% (n = 6) and inter-assay precision 1.95% (n = 12). The relative standard deviation percentage for accuracy was 1.28%. The recovery percentage was 101.5 ± 1.5%. LQ and LD were 2.18 µg/mL and 2.0 µg/mL respectively. The most destabilizing conditions were oxidizing and alkaline. The chromatograms confirmed no interference with the methadone signal. Conclusions The HPLC method has proved to be valid and reproducible for methadone quantification in a new oral solution with methylparaben and propylparaben. This assay is a rapid, simple and reliable technique that can be used in daily analysis and physicochemical stability studies.

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Determination of phenylethylamines in hallucinogenic cactus species by high-performance liquid chromatography with photodiode-array detection

Cited by 17 publications

References 13 publications

Analysis of 3,4-Methylenedioxymethamphetamine (MDMA) and its Metabolites in Plasma and Urine by HPLC-DAD and GC-MS

Analysis of 3,4-Methylenedioxymethamphetamine (MDMA) and its Metabolites in Plasma and Urine by HPLC-DAD and GC-MS

Identification and Individualization of Lophophora using DNA Analysis of the trnL/trnF Region and rbcL Gene

Development and validation of a HPLC-UV method for methadone hydrochloride quantification in a new oral solution with preservatives to be implemented in physicochemical stability studies

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