Improved sensitivity by use of gas chromatography—positive chemical ionization triple quadrupole mass spectrometry for the analysis of drug related substances

Gansbeke, Wim Van; Polet, Michaël; Hooghe, Fiona; Devos, Christophe; Eenoo, Peter Van

doi:10.1016/j.jchromb.2015.07.052

Cited by 25 publications

(40 citation statements)

References 21 publications

(25 reference statements)

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“…As described elsewhere, ammonia is used instead of methane as the reagent gas for all our analyses . The proton affinity of ammonia is higher than that of methane, causing less fragmentation and generating a larger proportion of the [M + H] + ion.…”

Section: Resultsmentioning

confidence: 99%

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Gas chromatography/chemical ionization triple quadrupole mass spectrometry analysis of anabolic steroids: ionization and collision‐induced dissociation behavior

Polet

Gansbeke

Eenoo

et al. 2016

Rapid Comm Mass Spectrometry

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Section: Resultsmentioning

confidence: 99%

“…Chemical ionization (CI) is a soft ionization technique and results, in comparison with EI, in fewer fragments with higher intensities, ideal for selection as precursor ions for MS/MS . GC/CI‐MS/MS also opens up new possibilities in the search for new metabolites.…”

mentioning

confidence: 99%

Gas chromatography/chemical ionization triple quadrupole mass spectrometry analysis of anabolic steroids: ionization and collision‐induced dissociation behavior

Polet

Gansbeke

Eenoo

et al. 2016

Rapid Comm Mass Spectrometry

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“…Eventually three metabolites (M6, M7 and M16) were chosen to be included in the routine screening method. Only the most important metabolites were selected to avoid overloading the screening method with transitions, as it already contained more than 250 compounds . This updated screening method has been used to analyze more than 9000 routine urine samples from athletes.…”

Section: Resultsmentioning

confidence: 99%

“…In 2015, a GC triple quadrupole MS method that used chemical ionization (CI), instead of electron ionization (EI) was introduced. A comparative study showed that GC‐CI‐MS/MS, in relation to GC‐EI‐MS/MS, significantly increased the sensitivity for a wide range of compounds . This GC‐CI‐MS/MS method also opened new possibilities in the search for new metabolites.…”

Section: Introductionmentioning

confidence: 99%

Efficient approach for the detection and identification of new androgenic metabolites by applying SRM GC‐CI‐MS/MS: a methandienone case study

et al. 2016

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Identification of anabolic androgenic steroids (AAS) is a vital issue in doping control and toxicology, and searching for metabolites with longer detection times remains an important task. Recently, a gas chromatography chemical ionization triple quadrupole mass spectrometry (GC-CI-MS/MS) method was introduced, and CI, in comparison with electron ionization (EI), proved to be capable of increasing the sensitivity significantly. In addition, correlations between AAS structure and fragmentation behavior could be revealed. This enables the search for previously unknown but expected metabolites by selection of their predicted transitions. The combination of both factors allows the setup of an efficient approach to search for new metabolites. The approach uses selected reaction monitoring which is inherently more sensitive than full scan or precursor ion scan. Additionally, structural information obtained from the structure specific CI fragmentation pattern facilitates metabolite identification. The procedure was demonstrated by a methandienone case study. Its metabolites have been studied extensively in the past, and this allowed an adequate evaluation of the efficiency of the approach. Thirty three metabolites were detected, including all relevant previously discovered metabolites. In our study, the previously reported long-term metabolite (18-nor-17β-hydroxymethyl,17α-methyl-androst-1,4,13-trien-3-one) could be detected up to 26 days by using GC-CI-MS/MS. The study proves the validity of the approach to search for metabolites of new synthetic AAS and new long-term metabolites of less studied AAS and illustrates the increase in sensitivity by using CI. Copyright © 2016 John Wiley & Sons, Ltd.

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“…The screening procedure offers the advantage of very short run times (5 min) and a minimalistic sample preparation consisting of a simple dilution step with subsequent addition of one ISTD. Using GC‐QqQ‐MS with chemical ionization (CI), 37 target analytes from the class of stimulants were (amongst other compounds) sensitively detected . The analytes were incorporated into established sample preparation protocols based on enzymatic hydrolysis, LLE, and trimethylsilylation prior to GC‐CI‐MS/MS measurement, and LODs between 2 and 100 ng/mL were accomplished, demonstrating the fitness‐for‐purpose for this test method.…”

Section: Stimulantsmentioning

confidence: 99%

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

Thevis

Kuuranne

Walpurgis

et al. 2016

Drug Testing and Analysis

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The aim of improving anti-doping efforts is predicated on several different pillars, including, amongst others, optimized analytical methods. These commonly result from exploiting most recent developments in analytical instrumentation as well as research data on elite athletes' physiology in general, and pharmacology, metabolism, elimination, and downstream effects of prohibited substances and methods of doping, in particular. The need for frequent and adequate adaptations of sports drug testing procedures has been incessant, largely due to the uninterrupted emergence of new chemical entities but also due to the apparent use of established or even obsolete drugs for reasons other than therapeutic means, such as assumed beneficial effects on endurance, strength, and regeneration capacities. Continuing the series of annual banned-substance reviews, literature concerning human sports drug testing published between October 2014 and September 2015 is summarized and reviewed in reference to the content of the 2015 Prohibited List as issued by the World Anti-Doping Agency (WADA), with particular emphasis on analytical approaches and their contribution to enhanced doping controls.

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Improved sensitivity by use of gas chromatography—positive chemical ionization triple quadrupole mass spectrometry for the analysis of drug related substances

Cited by 25 publications

References 21 publications

Gas chromatography/chemical ionization triple quadrupole mass spectrometry analysis of anabolic steroids: ionization and collision‐induced dissociation behavior

Gas chromatography/chemical ionization triple quadrupole mass spectrometry analysis of anabolic steroids: ionization and collision‐induced dissociation behavior

Efficient approach for the detection and identification of new androgenic metabolites by applying SRM GC‐CI‐MS/MS: a methandienone case study

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

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