OBJECTIVE: Synthetic cathi-nones (SCs) are new psychoactive substances with sympathomimetic effects, which emerged into the illegal drug market to replace con-trolled stimulants. Since every year more pow-erful and toxic substances enter the illicit mar-ket, there is the need for analytical methodol-ogies able to detect these new compounds in conventional and non-conventional biological matrices. We sought to develop and validate a targeted screening and quantification method for thirty-two parent SCs and two metabolites in hair samples by ultra-high-performance liq-uid chromatography coupled to high resolution mass spectrometry (UHPLC-HRMS).MATERIALS AND METHODS: 20 mg hair samples were soaked in 250 mu L of 2 mM ammo-nium formate, methanol and acetonitrile mix-ture (50/25/25, v/v/v) and incubated overnight at 40 degrees C. After incubation, the samples were evaporated to dryness under nitrogen stream and reconstituted with 100 mu L of mobile phase mix (A:B, 80:20) and 10 mu L were injected into UHPLC-HRMS. A Q ExactiveTM Focus Orbitrap Mass spectrometer with full scan and target-ed data-dependent MS/MS scan acquisition was used for the screening and quantitation analysis.RESULTS: The assay was linear from 5 to 500 pg/mg hair for all the analytes under inves-tigation. Intra-day and inter-day precision were always < 15% and matrix effect and analytical recovery were always within acceptable criteria (+/- 25% and >50%, respectively). The developed method was applied to authentic hair samples from SCs consumers. The most prevalent found SCs were 3,4-Methylenedioxy-alpha-Pyrrolidinohex-anophenone with a concentration range of 6.0-1,000.0 pg/mg along with alpha-Pyrrolidinohexio-phenone (54.0 and 554.0 pg/mg, respectively), 3-Methylmetcathinone (556.0 and 5,000.0 pg/ mg) and 4-Methylethcathinone (11.5 and 448.0 pg/mg)CONCLUSIONS: The developed method showed good selectivity, specificity, an easy and low-cost sample preparation and an analysis time compat-ible with a high throughput laboratory.
Targeted screening and quantification of synthetic cathinones and metabolites in hair by UHPLC-HRMS / La Maida, N; Mannocchi, G; Pichini, S; Basile, G; Di Giorgi, A; Busardò, F P; Marchei, E. - In: EUROPEAN REVIEW FOR MEDICAL AND PHARMACOLOGICAL SCIENCES. - ISSN 1128-3602. - 26:14(2022), pp. 5033-5042. [10.26355/eurrev_202207_29289]
Targeted screening and quantification of synthetic cathinones and metabolites in hair by UHPLC-HRMS
La Maida, N;Mannocchi, G;Pichini, S;Basile, G;Di Giorgi, A;Busardò, F P;
2022-01-01
Abstract
OBJECTIVE: Synthetic cathi-nones (SCs) are new psychoactive substances with sympathomimetic effects, which emerged into the illegal drug market to replace con-trolled stimulants. Since every year more pow-erful and toxic substances enter the illicit mar-ket, there is the need for analytical methodol-ogies able to detect these new compounds in conventional and non-conventional biological matrices. We sought to develop and validate a targeted screening and quantification method for thirty-two parent SCs and two metabolites in hair samples by ultra-high-performance liq-uid chromatography coupled to high resolution mass spectrometry (UHPLC-HRMS).MATERIALS AND METHODS: 20 mg hair samples were soaked in 250 mu L of 2 mM ammo-nium formate, methanol and acetonitrile mix-ture (50/25/25, v/v/v) and incubated overnight at 40 degrees C. After incubation, the samples were evaporated to dryness under nitrogen stream and reconstituted with 100 mu L of mobile phase mix (A:B, 80:20) and 10 mu L were injected into UHPLC-HRMS. A Q ExactiveTM Focus Orbitrap Mass spectrometer with full scan and target-ed data-dependent MS/MS scan acquisition was used for the screening and quantitation analysis.RESULTS: The assay was linear from 5 to 500 pg/mg hair for all the analytes under inves-tigation. Intra-day and inter-day precision were always < 15% and matrix effect and analytical recovery were always within acceptable criteria (+/- 25% and >50%, respectively). The developed method was applied to authentic hair samples from SCs consumers. The most prevalent found SCs were 3,4-Methylenedioxy-alpha-Pyrrolidinohex-anophenone with a concentration range of 6.0-1,000.0 pg/mg along with alpha-Pyrrolidinohexio-phenone (54.0 and 554.0 pg/mg, respectively), 3-Methylmetcathinone (556.0 and 5,000.0 pg/ mg) and 4-Methylethcathinone (11.5 and 448.0 pg/mg)CONCLUSIONS: The developed method showed good selectivity, specificity, an easy and low-cost sample preparation and an analysis time compat-ible with a high throughput laboratory.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
