Abstract:
:A microextraction by packed sorbent (MEPS) procedure for rapid concentration of methadone and its primary metabolite (EDDP) in hair samples was developed. The miniaturized approach coupled to gas chromatography with tandem mass spectrometry (GC-MS-MS) was successfully validated. Hair samples (50 mg) were incubated with 1 mL of 1 M sodium hydroxide for 45 min at 50°C, time after which the extract was neutralized by adding 100 μL of 20% formic acid. Subsequently, MEPS was applied using a M1 sorbent (4 mg; 80% C8 and 20% strong cation-exchange (SCX)), first conditioned with three 250-μL cycles of methanol and three 250-μL cycles of 2% formic acid. The extract load occurred with nine 150-μL cycles followed by a washing step involving three 50-μL cycles with 3.36% formic acid. For the elution of the analytes, six 100-μL cycles of 2.36% ammonium hydroxide in methanol were applied. The method was linear from 0.01 to 5 ng/mg, for both compounds, presenting determination coefficients greater than 0.99. Precision and accuracy were in accordance with the statements of international guidelines for method validation. This new miniaturized approach allowed obtaining recoveries ranging from 73 to 109% for methadone and 84 to 110% for EDDP, proving to be an excellent alternative to classic approaches, as well as other miniaturized procedures.
journal_name
J Anal Toxicoljournal_title
Journal of analytical toxicologyauthors
Rosado T,Gallardo E,Vieira DN,Barroso Mdoi
10.1093/jat/bkaa040subject
Has Abstractpub_date
2020-12-12 00:00:00pages
840-850issue
8eissn
0146-4760issn
1945-2403pii
5826077journal_volume
44pub_type
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