PMID- 29980017 OWN - NLM STAT- MEDLINE DCOM- 20181115 LR - 20181115 IS - 1873-264X (Electronic) IS - 0731-7085 (Linking) VI - 159 DP - 2018 Sep 10 TI - Iron oxide/silica/polypyrrole nanocomposite sorbent for the comparison study of direct-immersion and headspace solid-phase microextraction of aldehyde biomarkers in human urine. PG - 37-44 LID - S0731-7085(18)30679-4 [pii] LID - 10.1016/j.jpba.2018.06.052 [doi] AB - The short chain alkyl aldehydes, especially hexanal and heptanal, in urine are considered as potential biomarkers of several diseases and their determination in biological fluids has gained a great attention in recent years. Magnetic iron oxide core-shell silica (Fe(3)O(4)/SiO(2)) nanoparticles was synthesized and embedded in polypyrrole (PPy) during the in-situ electropolymerization on the surface of a stainless-steel wire. The Fe(3)O(4)/SiO(2)/PPy coated steel wire was used as a novel and effective solid-phase microextraction (SPME) fibre. It was employed for the extraction and preconcentration of hexanal and heptanal through direct-immersion (DI-) and headspace (HS-) SPME sampling strategies, followed by GC-FID quantification. The prepared nanocomposite fiber was characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR). All influential variables on the extraction efficiency of the DI- and HS-SPME sampling modes were studied and optimized. The calibration curves showed acceptable linearity (R(2) > 0.99) over the range of 0.01-10 mug mL(-1) for the DI-SPME-GC-FID and 0.01-15 mugmL(-1) for HS-SPME-GC-GID methods. The limit of detections (LODs) corresponding to the analytes amounts for which signal-to-noise ratios were equal to 3, estimated to be 0.1 and 0.5 ng mL(-1), for hexanal and heptanal using HS-SPME-GC-FID, respectively. The LODs for DI-SPME-GC-FID method were 0.1 and 1.0 for hexanal and heptanal. For six replicated analyses of 0.5 mug mL(-1) of the analytes, the relative standard deviations (RSDs) were calculated 6.5-6.6% and 5.1-5.3%, for DI-SPME and HS-SPME, respectively. The two developed methods were successfully applied for analysis of hexanal and heptanal in urine samples without derivatization step. The HS-SPME-GC-FID sampling/determination strategy showed better analytical figures of merit and longer lifetime for the prepared nanocomposite fiber. CI - Copyright (c) 2018 Elsevier B.V. All rights reserved. FAU - Ghiasvand, Alireza AU - Ghiasvand A AD - Department of Chemistry, Lorestan University, Khoramabad, Iran. Electronic address: a_ghiasvand@yahoo.com. FAU - Heidari, Nahid AU - Heidari N AD - Department of Chemistry, Lorestan University, Khoramabad, Iran. FAU - Abdolhosseini, Sana AU - Abdolhosseini S AD - Department of Chemistry, Lorestan University, Khoramabad, Iran. LA - eng PT - Comparative Study PT - Journal Article DEP - 20180628 PL - England TA - J Pharm Biomed Anal JT - Journal of pharmaceutical and biomedical analysis JID - 8309336 RN - 0 (Aldehydes) RN - 0 (Biomarkers) RN - 0 (Ferric Compounds) RN - 0 (Polymers) RN - 0 (Pyrroles) RN - 1K09F3G675 (ferric oxide) RN - 30604-81-0 (polypyrrole) RN - 7631-86-9 (Silicon Dioxide) SB - IM MH - Aldehydes/*urine MH - Biomarkers/urine MH - Ferric Compounds/*chemistry MH - Humans MH - Nanocomposites/*chemistry MH - Polymers/*chemistry MH - Pyrroles/*chemistry MH - Silicon Dioxide/*chemistry MH - Solid Phase Microextraction/*methods OTO - NOTNLM OT - Direct immersion solid-phase microextraction OT - Diseases biomarker OT - Fe(3)O(4)/SiO(2)/PPY nanocomposite OT - Headspace solid-phase microextraction OT - Heptanal OT - Hexanal EDAT- 2018/07/07 06:00 MHDA- 2018/11/16 06:00 CRDT- 2018/07/07 06:00 PHST- 2018/03/22 00:00 [received] PHST- 2018/05/25 00:00 [revised] PHST- 2018/06/25 00:00 [accepted] PHST- 2018/07/07 06:00 [pubmed] PHST- 2018/11/16 06:00 [medline] PHST- 2018/07/07 06:00 [entrez] AID - S0731-7085(18)30679-4 [pii] AID - 10.1016/j.jpba.2018.06.052 [doi] PST - ppublish SO - J Pharm Biomed Anal. 2018 Sep 10;159:37-44. doi: 10.1016/j.jpba.2018.06.052. Epub 2018 Jun 28.