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, February 2012, Pages 15–30
Identification of cathinones and other active components of &legal highs& by mass spectrometric methods,
Institute of Forensic Research, Department of Forensic Toxicology, Westerplatte 9, Krakow 31033, PolandThe supply of psychoactive substances has changed and users increasingly buy &legal highs& over the Internet or in specialized shops. Vast arrays of preparations are marketed as legal substitutes to controlled substances. Their analysis has revealed that the majority of active components belong to one of four chemical classes: phenethylamines, tryptamines, piperazines and cathinones, the last being novel.This article gives special attention to cathinone derivatives and certain characteristic fragmentations based on the GC-EI/MS and LC-ESI/QTOF-MS spectra. The parent ions of these substances are hard to obtain by EI/MS, whereas the protonated molecular ions can be observed clearly by ESI/QTOF-MS. Furthermore, two major characteristic α-cleavages are produced when the EI mode is used, leading to formation of iminium and acylium ions, respectively. These ions can process secondary and tertiary fragmentations, which are very useful in identification. In the case of ESI/QTOF-MS, characteristic fragments are produced via loss of water in cathinones, being secondary amines.The targeted MS/MS mode allows us to identify structures of many unknown substances with certainty. Nevertheless, in order to determine the location of a substituent in a molecule, it is sometimes necessary to use NMR or FTIR.Problems found in identifying novel recreational drugs sold as &legal highs& indicate the need for international collaboration and sharing knowledge and analytical data amongst experts from forensic and clinical laboratories.Highlights? I analyzed mass spectral behaviors of substances found in &legal highs&. ? A general scheme for identifying chemical class of unknown substance uses GC-EI/MS. ? I discussed the fragmentation of cathinones under EI/MS and ESI/QTOF-MS.Abbreviations2,3-DCPP, 1-(2,3-dichlorophenyl)piperazine; 2C-B-BZP, 1-(4-bromo-2,5-dimethoxybenzyl)piperazine; 3,4-DMMC, 3,4-dimethylmethcathinone; 4-MEC, 4-methylethylcathinone; 5-MeO-α,N-DMT, 5-methoxy-α,N-dimethyltryptamine; AMT, α-methyltryptamine; Buphedrone, α-methylamino-butyrophenone or 2-(methylamino)-1-phenylbutan-1-one; Bupropion, 2-(tert-butylamino)-1-(3-chlorophenyl)propan-1-one; Butylone, β-keto-N-methylbenzodioxolylpropylamine; BZP, 1-benzylpiperazine; DBZP, 1,4-dibenzylpiperazine (dibenzylpiperazine); Diethylpropion, N,N-diethylcathinone (Amfepramone); DMMC, N,N-dimethylmethcathinone; Ethcathinone, N-ethylcathinone; Ethylone, 3,4-methylenedioxy-N-ethylcathinone; Flephedrone, 4-fluoromethcathinone; MBZP, 1-benzyl-4-methylpiperazine; mCPP, 1-(3-chlorophenyl)piperazine (meta-chlorophenylpiperazine); MDPBP, 3,4-methylenedioxypyrrolidin-1-ynbutiophenone; MDPPP, 3,4-methylenedioxy-pyrrolidin-1-ynpropiophenone; MDPV, 3,4-methylenedioxypyrrolidin-1-ynvalerone; MeOPP, 1-(4-methoxyphenyl)piperazine (methoxyphenylpiperazine); Mephedrone, 4-methylmethcathinone; Methcathinone, N-methylcathinone; Methedrone, 4-methoxymethcathinone; Methylone, 3,4-methyleneedioxymethcathinone; MoPPP, 4-methoxy-pyrrolidin-1-ynpropiophenone; MPBP, 4-methylpyrrolidin-1-ynbutiophenone; MPPP, 4-methyl-pyrrolidin-1-ynpropiophenone; Naphyrone, 1-naphthalen-2-yl-2-pyrrolidin-1-ylpentan-1-one; PAPP, α-phthalimidopropiophenone; Pentedrone, 1-phenyl-2-methylamino-pentan-1-one; Pentylone, β-keto-3,4-methylbenzodioxolylpentanamine; pFPP, 1-(4-fluorophenyl)piperazine (para-fluorophenylpiperazine); PMMA, p-methoxymethamphetamine; PPP, Pyrrolidin-1-ynpropiophenone; PVP, Pyrrolidin-1-ynvalerophenone; TFMPP, 1-(3-trifluoromethylphenyl)piperazineKeywordsα-cleavage; Active component; Cathinone; Characteristic fragmentation; Identification; Legal high; Mass spectrometry; Parent ion; Protonated molecular ion; Recreational drug
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, 4 January 2007, Pages 73–82
Optimization of GC&MS conditions based on resolution and stability of analytes for simultaneous determination of nine sesquiterpenoids in three species of Curcuma rhizomes, , , , ,
Institute of Chinese Medical Sciences, University of Macau, Taipa, MacauGC&MS is a powerful tool for analysis of volatile oil, and resolutions of analytes were exclusively used as marker for optimization of the conditions. However, volatile oil usually contains heat labile components which may degrade and result in wrong results during GC analysis. In present study, based on both resolutions and stabilities of 11 sesquiterpenoids, GC&MS conditions were optimized for simultaneously quantitative determination of nine compounds including β-elemene, curzerene, curcumol, isocurcumenol, germacrone, curdione, curcumenol, neocurdione and curcumenone in Ezhu. However, the other two compounds, i.e. furanodienone and furanodiene, were still thermal sensitive and not available for GC analysis. The results showed that both resolutions and stabilities of analytes should be considered for optimization of GC conditions because the properties of most components in volatile oil are unknown. Under optimum conditions, a capillary column (30 m & 0.25 mm i.d.) coated with 0.25 μm film 5% phenyl methyl siloxane was used for separation. Pulsed splitless inlet with temperature of 190 &C was selected for sample injection (0.2 μl). The calibration curves of nine sesquiterpenoids showed good linearity (r2 & 0.9989) within test ranges. The optimized method showed good repeatability for quantification of these nine components in Ezhu with intra- and inter-day variations of less than 1.42% and 2.79%, respectively. The validated method was successfully applied to quantify 9 sesquiterpenoids in 18 samples of 3 species of Curcuma used as Ezhu.KeywordsGas chromatography&mass spectrometry; Sesquiterpenoids; Resolution; Stability; Pressurized liquid extraction; Curcuma
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Available online 26 October 2016 —
Characterization and quantification of poly(acrylonitrile-co-1,3-butadiene-co-styrene)/polyamide 6 (ABS/PA6) blends using pyrolysis-gas chromatography (Py-GC) with different detector systems, , , , , , a Bonn-Rhein-Sieg University of Applied Sciences, Department of Applied Natural Sciences, von-Liebig-Str. 20, 53359 Rheinbach, Germanyb AKRO-PLASTIC GmbH, Im Stiefelfeld 1, 56651 Niederzissen, Germany&Characterization of poly(acrylonitrile-co-1,3-butadiene-co-styrene) (ABS) and polyamide 6 (PA 6) blends by analytical pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) and analytical pyrolysis-gas chromatography with flame ionization detector (Py-GC/FID).&Successfully validation of the developed Py-GC/MS method on the quantification of the PA 6 amount (%, w/w) of the investigated blend-standards.&Quantification of the PA 6 and ABS amount (%, w/w) of the investigated blend standards.Solid blend samples of poly(acrylonitrile-co-1,3-butadiene-co-styrene) (ABS) and polyamide 6 (PA 6) were characterized by analytical pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) and analytical pyrolysis-gas chromatography with flame ionization detector (Py-GC/FID) at 700 &C, respectively. The separated compounds were identified using the mass spectral library as well as by calculation of the relative retentions. These blends have been chosen, since they play a dominant role in the automotive and other industries.A sixfold determination of the polymer blends was carried out respectively with both Py-GC/MS and Py-GC/FID methods. After characterization of the pyrolysis products, peak area ratios of five major degradation products were determined. Eventually, the obtained analytical results were then used to compare the precision of both Py-GC/MS and Py-GC/FID methods. Their relative standard deviations (RSD) of the determined peak area ratios were therefore compared. The performed statistical tests led to the conclusion that the Py-GC/FID method is more suitable for the quantification purposes than the Py-GC/MS method. Afterwards, the Py-GC/FID method has been validated successfully on the quantification of PA 6, using the peak area ratio of caprolactam to the main ABS degradation products. For the method validation the parameters linearity and working range, accuracy, limits of detection (LOD) and quantification (LOQ), and the recoveries, have been determined. A LOD of 6.02 (%, w/w) and a LOQ of 18.1 (%, w/w) were calculated. The recoveries for two blend-standards in the low and high content range were 100% and 97.7%, respectively. The calculated recovery of the investigated unknown sample was 93.3%.KeywordsPyrolysis-GC/FID; Pyrolysis-GC/MS; Poly(acrylonitrile-co-1,3-butadiene-co-styrene)/polyamide 6 (ABS/PA 6) blends; Quantification; Method validation
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, December 2016, Pages 71–74
Open Access
Case ReportThe first Mongolian cases of phenylketonuria in selective screening of inborn errors of metabolism, , , , , , , , , , a Chidlren's Hospital, National Center for Maternal and Child Health, Bayangol district, Ulaanbaatar 16060, Mongoliab Department of Pediatrics, Shimane University School of Medicine, 89-1 Enya, Izumo, Shimane 693-8501, Japanc Department of Pediatrics, Osaka City University Graduate School of Medicine, 1-4-3 Asahi-machi, Abeno-ku, Osaka 545-8585, JapanBackgroundInborn errors of metabolism (IEM) are rare genetic disorders in which a single gene defect causes a clinically significant block in a metabolic pathway. Clinical problems arise due to either accumulation of substrates that are toxic or interfere with normal function, or deficiency of the products that are used to synthesize essential compounds. There is no report of screening results or confirmed cases of IEM in Mongolia. Only pilot study of newborn screening for congenital hypothyroidism was implemented in Mongolia, where the incidence of congenital hypothyroidism is calculated to be 1:3057 in Mongolia.MethodsTwo hundred twenty-three Mongolian patients, who had developmental delay, psychomotor retardation with unknown cause, seizures, hypotonia or liver dysfunction, were studied. Urinary organic acid analysis was performed in all cases using gas chromatography mass spectrometric (GC/MS) analysis. Blood amino acids and acylcarnitines were checked in the patients who had abnormal GC/MS analyses. Mutation analysis was done in the patients, who were suspected having specific inborn errors of metabolism by mass spectrometric analysis.ResultsOne hundred thirty-nine children had normal urinary organic acid analyses. Thirty one had metabolites of valproic acid, 17 had non- or hypoketotic dicarboxylic aciduria, 14 had tyrosiluria, 12 had ketosis, 4 had elevation of lactate and pyruvate, 3 had increased excretion of urinary glycerol or methylmalonic acids, respectively, and 2 had elevation of phenylacetate and phenyllactate. We checked blood amino acids and acylcarnitines in 38 patients, which revealed phenylketonuria (PKU) in 2 patients, and one with suspected citrin deficiency. Mutation analysis in PAH was done in 2 patients with PKU, and previously reported p.R243Q, p.Y356X, p.V399V, p.A403V mutations were detected.DiscussionIn conclusion, these were the first genetically confirmed cases of PKU in Mongolia, and the study suggested that the newborn screening program for PKU was significant because it enabled early treatment dietary restriction, specialized formulas and other medical management for prevention of neurological handicaps in these children.KeywordsPhenylketonuria; Inborn errors of metabolism; Mongolia; Screening1. IntroductionInborn errors of metabolism (IEM) are rare genetic disorders caused by a single gene defect, resulting in metabolic disarrangements and neurological handicaps in children. Clinical problems arise due to accumulation of the upstream substrates which are toxic or interfere with normal function, or deficit of the products which are used to synthesize essential compounds or energy. The major groups of IEMs included organic acidemias, aminoacidopathies, fatty acid oxidation disorders, disorders of carbohydrate metabolism, or accumulative disorders such as lysosomal diseases, and so on. First discovered were aminoacidopathies such as alkaptonuria in 1891 and phenylketonuria in 1937. When metabolic disorders are diagnosed in early infancy, treatment can commence immediately, preventing irreversible damage and life-threatening illnesses.Initially, phenylketonuria (PKU) was screened in newborns by a bacterial inhibition assay pioneered in 1961 by Guthrie , and subsequently other IEMs were added to the target panel of newborn screening using tandem mass spectrometry (MS/MS). Patients with PKU show high levels of phenylalanine in the blood and consequently suffer from neurological impairment. Phenylalanine in high levels is toxic to the brain, therefore, untreated patients with PKU show mental retardation, convulsions, or behavioral abnormalities. In order to prevent children from such damage, the patients must be diagnosed early and follow a lifelong phenylalanine restricted diet. Munkhtuvshin et al.
performed the Guthrie test in 620 children aged 8 to 18 years with diagnosis of oligophrenia for purpose of detecting PKU, and 10 (1.63%) patients had elevated phenylalanine (higher than 4 mg/dl), although enzyme assay and mutation analysis were not performed (report in Mongolian).There have never been reports confirmed cases of inborn errors of metabolism such as organic acidemias, aminoacidopathies or fatty acid oxidation disorders in Mongolia. A pilot study of newborn screening for congenital hypothyroidism was implemented in Mongolia, and the incidence of congenital hypothyroidism is calculated to be 1:3057 in Mongolia . We screened urinary organic metabolites in 223 children with developmental delay and psychomotor retardation using GC/MS to determine IEM in Mongolian children.2. Subjects and methods<h3 class="svArticle" id="s. SubjectsWe analyzed urine samples from 223 Mongolian children (124 boys and 99 girls) who had clinical symptoms such as developmental delay, psychomotor retardation, seizures and hypotonia between 2014 and 2015. The children were from 1 day to 16 years of age. There were no patients from consanguineous marriage. 19 patients had family history of similar clinical signs and psychomotor retardation in her/his siblings or relatives. Urinary organic acid analysis was performed in all cases using GC/MS analysis, and blood amino acids and acylcarnitines levels were checked by MS/MS on the patients who had abnormality in GC/MS analysis for confirmation of fatty acid oxidation disorders. Mutation analysis was done in the patients, who were suspected of having specific inborn errors of metabolism. Informed consent for study was obtained from the parents of the patients. This study was approved by the Ethical Committee of the Ministry of Health in Mongolia.<h3 class="svArticle" id="s. Methods<h4 class="svArticle" id="s.1. Urinary organic acid analysis.Urinary organic acid and blood acylcarnitine analyses were performed at the Shimane University Faculty of Medicine, Shimane Prefecture, Japan. Extracts of urine in the filter paper (50 & 50 mm, Advantec 327) containing 0.2 mg of creatinine were analyzed with oximation, solvent extraction, and derivatization as described  and  using capillary GC/MS QP 2010 PLUS system (Shimadzu, Kyoto, Japan). The capillary column was a fused silica DB-5 column (30 m & 0.25 mm i.d.) with a 1-μm-thick 5% phenylmethyl silicone film (J & W Scientific, Folsom, CA, USA). The internal standards comprised 20 μg each of heptadecanoic acid (HDA) and tetracosane (C24), as well as 40 μg of tropic acid (TA). The unit of organic acid compounds was described as relative peak area (RPA, %) to the area of internal standard (heptadecanoic acid).<h4 class="svArticle" id="s.2. Blood amino acid and acylcarnitine analysis using MS/MSBlood amino acids and acylcarnitines were analyzed using MS/MS (API 3000; Applied Biosystems, Foster City, CA, USA, and Shimadzu LC-MSMS 8030, Shimadzu, Kyoto, Japan). 200 μl of methanol including an isotope-labeled internal standard (Cambridge Isotope Laboratories, Kit NSK-A/B, Cambridge, UK) was added to aliquots of blood filter paper. Supernatant aliquots were dried under a nitrogen stream, and butylated with 50 μl of 3 N n-butanol-HCl at 65 &C for 15 min. The dried butylated sample was dissolved in 100 μl of 80% acetonitrile:water (4:1 v/v) and then the amino acids and acylcarnitines were determined using MS/MS and quantified using ChemoView& software (Applied Biosystems/MDS SCIEX, Toronto, Canada) .<h4 class="svArticle" id="s.3. Mutation analysisGenomic DNA was extracted from the patients and their parents' peripheral blood lymphocytes using the QIAamp DNA Micro Kit (Qiagen GmbH, Hilden, Germany). Mutation analysis was performed in the Department of Pediatrics, Osaka City University Graduate School of Medicine, Japan. Thirteen sets of primers were designed for the amplification of each exon including 5& and 3& splice sites of the phenylalanine hydroxylase (PAH) gene. Exons were amplified for 35 cycles using the polymerase chain reaction (PCR) as follows: denaturation at 95 &C for 30 s, annealing at 55 &C for 30 s, and extension at 72 &C for 30 s with the AmpliTaq Gold PCR Master Mix (Applied Biosystems, Foster City, CA, USA) using the iCycler (Bio Rad Laboratories Inc., Hercules, CA, USA). All PCR-amplified fragments of PAH were then directly sequenced using ABI Big Dye Terminator Cycle Sequencing FS Ready Reaction Kits and an ABI PRISM 310 Genetic Analyzer (Applied Biosystems).3. ResultsThe clinical findings included 108 with developmental delay, 96 with seizures, 87 with mental retardation, 81 with hypotonia, 46 with congenital anomalies, 39 with lethargy, 37 with apnea/dyspnea, 34 with hepatomegaly, 33 with acute encephalopathy, 33 with vomiting, 15 with muscle pain, 10 with coma and 10 with cardiomyopathy, respectively.The urinary organic acid analysis was normal in 139 children. The following metabolic abnormalities were detected in others: 31 patients who had a history of convulsions treated with valproic acid had metabolites of valproic acid, 17 had non- or hypoketotic dicarboxylic aciduria, 14 had tyrosiluria, 12 had ketosis, 4 had elevation of lactate and pyruvate, 3 had increased excretion of urinary glycerol or methylmalonic acids, respectively, and 2 had elevated levels of phenylacetatic and phenyllactic acids.
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