Sensitive, rapid and validated gas chromatography/negative ion chemical ionization-mass spectrometry assay including derivatisation with a novel chiral agent for the enantioselective quantification of amphetamine-type stimulants in hair☆

IFentanyl is a synthetic opioid used to treat intense chronic pain. In this study, the authors report detection and quantification of fentanyl in sweat and hair of a patient receiving fentanyl (25 pg/h) via a transdermal therapeutic system (TTS) for 22 days. Sweat was collected using sweat patches every night on days 13-21 of the therapy, and hair was collected 12 weeks after the end of the treatment. Detection and quantification was performed wffh liquid chromatography-tandem mass spectrometry using electron spray ionization in selected reaclion monitoring mode. Alfentanyl was used as internal standard for quantification in hair and in sweat. Sodium ions have been used as endogenous internal reference for determination of volume of sweat excreted on each patch. Results show presence of fentanyl in both matrices. Fentanyl concentrations in sweat varied from 0.17 to 1.02 ng/pL, and timeresolved segmented hair analysis showed a maximum fentanyl concentration of 0.48 ng/mg of hair during the period of the therapy.

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“…The second extracts thus corresponded to 100% extraction efficiency. The ratio of the two results gave the extraction yield (29,30).…”

Section: Table I Hplc Separation Conditions For Lc-ms-ms Experimentsmentioning

confidence: 99%

Determination of Fentanyl in Sweat and Hair of a Patient using Transdermal Patches

Schneider

Ait-m-bark

Schummer

et al. 2008

Journal of Analytical Toxicology

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“…The hair pre-treatments and the derivatization procedure were realized according to the methods described by Martins et al [22,25].…”

Section: Sample Preparationmentioning

confidence: 99%

“…Drug enantiomers were converted into their diastereomeric derivatives by dissolving the dry residue into 200 mL of an 5% aqueous carbonate buffer (70 g/ L NaHCO 3 -30 g/L Na 2 CO 3 ; pH 9.5) followed by the addition of 20 mL of a 0.2 M solution of (S,R)-HFBOPCl [22]. The mixture was left on a rotary shaker at room temperature for 15 min.…”

Section: Sample Preparationmentioning

confidence: 99%

“…Tagliaro et al analyzed one hair specimen obtained from a single real ecstasy user by capillary electrophoresis (CE) and observed a predominance of the (R)-MDMA, while the electropherogram of its metabolite MDA clearly showed comparable enantiomeric concentrations [21]. Martins et al observed also in one hair specimen an R versus S ratio > 1 for MDMA and R/S ratio < 1 for its metabolite MDA [22]. Additionally, to the best of our knowledge, no data about the enantioselective disposition of MDMA and MDA in human segmented hair have been published yet.…”

Section: Introductionmentioning

confidence: 99%

“…All chemicals were of analytical grade. The derivatization reagent (2S,4R)-N-heptafluorobutyryl-4-heptafluorobutoyloxy-prolyl chloride [(S,R)-HFBOPCl] was synthesized according to the literature [22].…”

Section: Introductionmentioning

confidence: 99%

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