PMID- 17318511 OWN - NLM STAT- MEDLINE DCOM- 20070618 LR - 20160512 IS - 1618-2642 (Print) IS - 1618-2642 (Linking) VI - 388 IP - 2 DP - 2007 May TI - Determination of major and trace elements in human scalp hair by pressurized-liquid extraction with acetic acid and inductively coupled plasma-optical-emission spectrometry. PG - 441-9 AB - An analytical method has been developed for determination of major (Ca, K, Mg, and Na) and trace elements (As, Cd, Co, Li, Ni, and Sr) in human scalp hair. The proposed method includes a novel, simple, rapid, highly efficient, and automated metal-leaching procedure, by pressurized-liquid extraction (PLE), combined with a rapid simultaneous detection system-inductively coupled plasma-optical-emission spectrometry (ICP-OES). PLE is one of the most promising recently introduced sample-preparation techniques, with the advantages of reducing solvent consumption and enabling automated sample handling. The operating conditions for PLE, including concentration of the extraction solvent, extraction temperature, static time, number of extraction steps, pressure, mean particle size, diatomaceous earth (DE) mass/sample mass ratio, and flush volume were studied using an experimental design (Plackett-Burman design, PBD). The optimum conditions were use of 0.75 mol L-1 acetic acid as extracting solution and powdered hair samples thoroughly mixed with DE, as a dispersing agent, at a DE mass/sample mass ratio of 4. Extraction was performed at room temperature and an extraction pressure of 140 atm for 5 min in one extraction step. The flush volume was fixed at 60%. The PLE-assisted multi-element leaching proposed is complete after 7 min (5 min static time plus 1 min purge time plus 1 min end relief time). Under the optimised conditions the figures of merit, for example limits of detection and quantification, repeatability of the over-all procedure, and accuracy, were evaluated. Analysis of GBW-07601 (human hair) certified reference material revealed accuracy was good for the target elements. The optimised method was finally applied to several human scalp-hair samples. FAU - Moreda-Pineiro, Jorge AU - Moreda-Pineiro J AD - Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira s/n, 15071, A Coruna, Spain. jmoreda@udc.es FAU - Alonso-Rodriguez, Elia AU - Alonso-Rodriguez E FAU - Lopez-Mahia, Purificacion AU - Lopez-Mahia P FAU - Muniategui-Lorenzo, Soledad AU - Muniategui-Lorenzo S FAU - Prada-Rodriguez, Dario AU - Prada-Rodriguez D FAU - Moreda-Pineiro, Antonio AU - Moreda-Pineiro A FAU - Bermejo-Barrera, Pilar AU - Bermejo-Barrera P LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20070223 PL - Germany TA - Anal Bioanal Chem JT - Analytical and bioanalytical chemistry JID - 101134327 RN - 0 (Elements) RN - 0 (Trace Elements) RN - 61790-53-2 (Diatomaceous Earth) RN - Q40Q9N063P (Acetic Acid) SB - IM MH - Acetic Acid/*chemistry MH - Diatomaceous Earth MH - *Elements MH - Hair/*chemistry MH - Humans MH - Particle Size MH - Pressure MH - Reproducibility of Results MH - *Scalp MH - Spectrophotometry/*methods MH - Temperature MH - Trace Elements/*analysis/isolation & purification EDAT- 2007/02/24 09:00 MHDA- 2007/06/19 09:00 CRDT- 2007/02/24 09:00 PHST- 2006/09/25 00:00 [received] PHST- 2007/02/01 00:00 [accepted] PHST- 2007/01/22 00:00 [revised] PHST- 2007/02/24 09:00 [pubmed] PHST- 2007/06/19 09:00 [medline] PHST- 2007/02/24 09:00 [entrez] AID - 10.1007/s00216-007-1179-1 [doi] PST - ppublish SO - Anal Bioanal Chem. 2007 May;388(2):441-9. doi: 10.1007/s00216-007-1179-1. Epub 2007 Feb 23.