Microwave irradiation for a fast gas chromatography–mass spectrometric analysis of polysaccharide-based plasma volume expanders in human urine

Mazzarino, Monica; Angelis, Francesca De; Cicco, Teresa Di; Torre, Xavier de la; Botrè, Francesco

doi:10.1016/j.jchromb.2010.08.046

Cited by 8 publications

(8 citation statements)

References 24 publications

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“…The lowest level detectable in urine sample was 100 µg/ml for dextran and higher than 200 µg/ml (the limit of detection of the GC‐MS method currently used by the accredited anti‐doping laboratory of Rome) for HES.…”

Section: Introductionmentioning

confidence: 97%

A rapid analytical method for the detection of plasma volume expanders and mannitol based on the urinary saccharides and polyalcohols profile

Mazzarino

Fiacco

Torre

et al. 2011

Drug Testing and Analysis

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A screening procedure specifically developed for the detection of saccharides and polyalcohols in human urine in the framework of doping control analysis is presented. The proposed method, set-up, and validated to detect the abuse of dextran, hydroxyethyl starch and mannitol as a doping practice in sport, involves only one enzymatic hydrolysis step and the direct injection into a liquid chromatography-tandem mass spectrometry (LC-MS/MS) system. The chromatographic conditions were optimized to allow the efficient separation of compounds with the same molecular weight. Good linearity (R(2) 0.990-0.995) and reproducibility of relative retention times (CV% lower than 1) and of relative abundances of characteristic ion transitions (CV% lower than 10) were obtained. The lower limits of detection and quantification were in the range of 30-100 µg/ml. Since the analytes studied are present also in non-doping products (e.g. in fruit as well as in food products and drugs additives), the developed method was also used to establish a range of reference urinary concentrations: 600 doping control samples and 30 samples from volunteers not using any medication were considered. While the hydrolysis products (isomaltose and maltose hydroxyl-ethylated), used as specific markers for the detection of dextran and hydroxyethyl starch abuse, were not detected in urine; mannitol was present in all urines in a concentration range of 30-1200 µg/ml. Since no criteria of positivity for mannitol has been established yet, the results obtained in this study could be considered, in combination with those of previous researches, as a starting point to fix a threshold value for doping control purpose.

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Section: Introductionmentioning

confidence: 97%

A rapid analytical method for the detection of plasma volume expanders and mannitol based on the urinary saccharides and polyalcohols profile

Mazzarino

Fiacco

Torre

et al. 2011

Drug Testing and Analysis

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“…The optimization of microwave-assisted hydrolysis and derivatization of hydroxyethylstarch showed that hydrolysis could be finished in 2 min at 1,200 W, 100 o C and derivatization could be achieved within 5 min at 1,020 W, 100 o C. The sample preparation time is greatly shortened by this procedure, compared with traditional hydrolysis and derivatization (73). It should be noted that optimization procedure should be carefully carried out to avoid the degradation of monosaccharides during the hydrolysis.…”

Section: Acidic Hydrolysismentioning

confidence: 99%

Quality control of sweet medicines based on gas chromatography-mass spectrometry

Zhao

et al. 2015

DD&T

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“…While most of these are commonly combined in multi‐analyte screening methods, plasma volume expanders, which accounted for seven of the abovementioned positive test results, are frequently measured by dedicated procedures due to their physicochemical properties that are considerably different from most other masking agents. In order to accelerate the sample preparation for a GC‐MS‐based methodology concerning the detection of hydroxyethyl starch (HES), the utility of microwave irradiation in hydrolysis and derivatization was evaluated . Compared to conventional approaches, microwave‐assisted sample preparation shortened the hydrolysis and chemical derivatization time by more than 80 min, enabling faster reporting and more efficient use of available instrumental resources.…”

Section: Diuretics and Other Masking Agentsmentioning

confidence: 99%

“…In order to accelerate the sample preparation for a GC-MS-based methodology concerning the detection of hydroxyethyl starch (HES), the utility of microwave irradiation in hydrolysis and derivatization was evaluated. [83] Compared to conventional approaches, microwave-assisted sample preparation shortened the hydrolysis and chemical derivatization time by more than 80 min, enabling faster reporting and more efficient use of available instrumental resources. Targeting the same class of substances, i.e.…”

Section: Diuretics and Other Masking Agentsmentioning

confidence: 99%

Annual banned‐substance review: analytical approaches in human sports drug testing

Thevis

Kuuranne

Geyer

et al. 2012

Drug Testing and Analysis

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a International anti-doping efforts are harmonized and regulated under the umbrella of the World Anti-Doping Code and the corresponding Prohibited List, issued annually by the World Anti-Doping Agency (WADA). The necessity for a frequent and timely update of the Prohibited List (as the result of a comprehensive consultation process and subsequent consensual agreement by expert panels regarding substances and methods of performance manipulation in sports) is due to the constantly growing market of emerging therapeutics and thus new options for cheating athletes to illicitly enhance performance. In addition, 'tailor-made' substances arguably designed to undermine sports drug testing procedures are considered and the potential of established drugs to represent a doping substance is revisited in light of recently generated information. The purpose of the annual banned substance review is to support doping controls by reporting emerging and advancing methods dedicated to the detection of known and recently outlawed substances. This review surveys new and/or enhanced procedures and techniques of doping analysis together with information relevant to doping controls that has been published in the literature between October

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Microwave irradiation for a fast gas chromatography–mass spectrometric analysis of polysaccharide-based plasma volume expanders in human urine

Cited by 8 publications

References 24 publications

A rapid analytical method for the detection of plasma volume expanders and mannitol based on the urinary saccharides and polyalcohols profile

A rapid analytical method for the detection of plasma volume expanders and mannitol based on the urinary saccharides and polyalcohols profile

Quality control of sweet medicines based on gas chromatography-mass spectrometry

Annual banned‐substance review: analytical approaches in human sports drug testing

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