Determination of Phenolalkylamines, Narcotic Analgesics, and Beta-Blockers by Gas Chromatography/Mass Spectrometry

Lho, Dong-Seok; Hong, Jongki; Paek, Heang-Kee; Lee, Jeong-Ae; Park, Jongsei

doi:10.1093/jat/14.2.77

Cited by 37 publications

(13 citation statements)

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“…18,19 In this study, the derivatization of CAs by two step reaction exhibited a reasonable resolution and sensitivity except for dopa, as shown in Figure 2-(C). The base peaks of OTMS, NTFA (or NHFBA) derivatives are produced at m/z 267 or 355 by benzylic cleavage to form a stable ion, as shown in Figure 3.…”

Section: Methodssupporting

confidence: 56%

Chemical Derivatization of Catecholamines for Gas Chromatography-Mass Spectrometry

Park¹,

Kang²,

Li³

et al. 2009

Bulletin of the Korean Chemical Society

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GC/MS analysis of catecholamines (CAs) in biological sample may produce poor reproducible quantitaion when chemical derivatization is used as the technique to form a volatile derivative. Significant quantities of the side products can be formed from CAs with primary amine during the derivatization reaction under un-optimized conditions. We have tested various chemical derivatization techniques in an attempt to find an optimum derivatization method that will reduce side product formation, enable to separate several catecholamine derivatives in GC chromatogram, and obtain significant improvement of detection sensitivity in GC/MS analysis. Whereas several derivatization techniques such as trimethylsilylation (TMS), trifluoroacylation (TFA), and two step derivatization methods were active, selective derivatization to form O-TMS, N-heptafluorobutylacyl (HFBA) derivative using N-methyl-N-(trimethylsilyl)-trifluoroacetamide (MSTFA) and N-methyl-bis(heptafluorobutyramide) (MBHFBA) reagents was found to be the most effective method. Moreover, this derivative formed by selective derivatization could provide sufficient sensitivity and peak separation as well as produce higher mass ion as base peak to use selected ion in SIM mode. Calibration curves based on the use of an isotopically labeled internal standard show good linearity over the range assayed, 1 ~ 5000 ng/mL, with correlation coefficients of > 0.996. The detection limits of the method ranged from 0.2 to 5.0 ppb for the different CAs studied. The developed method will be applied to the analysis of various CAs in biological sample, combined with appropriate sample pretreatment.

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Section: Methodssupporting

confidence: 56%

Chemical Derivatization of Catecholamines for Gas Chromatography-Mass Spectrometry

Park¹,

Kang²,

Li³

et al. 2009

Bulletin of the Korean Chemical Society

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“…So far, there are several methods for determining PE in plasma, urine or tablet, such as gas chromatography (GC), 8 HPLC, 9 and GC-mass spectrometry (MS). 10 Most of these methods require a pretreatment of the separation steps and elaborate instruments.…”

Section: Introductionmentioning

confidence: 99%

An Electrochemical Sensor for Phenylephrine Based on Molecular Imprinting

et al. 2009

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Molecularly imprinted polymers (MIPs) were applied as molecular recognition elements to an electrochemical sensor for phenylephrine. A MIPs membrane was created on a glassy carbon electrode. SEM revealed a gradual change on the morphology of modified electrodes as the ratios of function monomer and cross-linking varied. When the ratio was 4:40, the surface morphology between the imprinted electrode (M-electrode) and the control electrode (N-electrode) became unambiguously different. This artificial receptor exhibited high selectivity for the template compared to closely related analogue. The response of the sensor varied in different concentration range might due to the heterogeneity of the MIPs membrane. This sensor was also used to determine phenylephrine in tablet samples.

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“…In the preparations for the Olympic Games in 1988, a laboratory in Seoul actively developed the method of gas chromatography-mass spectrometry for stimulants and narcotics 14,15 . Moreover, the abuse of beta-blockers was monitored for the first time using the improved method of gas chromatographymass spectrometry in the selected ion-monitoring regime, as well as diuretic abuse, using high-performance liquid chromatography.…”

Section: Improvement Of Analytical Methods For Anti-doping Controlmentioning

confidence: 99%

Historical development of analytical methods for anti-doping control

Stojanović¹,

Radovanović²

2017

Fizičko vaspitanje i sport kroz vekove

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SUMMARYAlthough the fight against the use of doping in sport has been going on for almost 90 years, its effects have become tangible in the last 45 years only, thanks to the use of valid and sensitive analytical methods. Historically, extensive international scientific cooperation and technological progress have laid down the basis for the development of high quality doping control laboratories worldwide. New biotechnology products are constantly being discovered and are made available on the doping market, so that anti-doping approaches must be raised to a higher level, and analytical methods must be constantly improved and refined, since it has bacome obvious that to some extent they lag behind new sophisticated doping agents. However, all the methods must first be scientifically proven and tested in order to be adequately used against doping in sport. If the technology and systematic use of the latest scientific anti-doping knowledge continue to develop and advance, it will greatly contribute to the development of analytical methods.

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Determination of Phenolalkylamines, Narcotic Analgesics, and Beta-Blockers by Gas Chromatography/Mass Spectrometry

Cited by 37 publications

References 0 publications

Chemical Derivatization of Catecholamines for Gas Chromatography-Mass Spectrometry

Chemical Derivatization of Catecholamines for Gas Chromatography-Mass Spectrometry

An Electrochemical Sensor for Phenylephrine Based on Molecular Imprinting

Historical development of analytical methods for anti-doping control

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