PMID- 26210111 OWN - NLM STAT- MEDLINE DCOM- 20151201 LR - 20150811 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1409 DP - 2015 Aug 28 TI - A salting out system for improving the efficiency of the headspace solid-phase microextraction of short and medium chain free fatty acids. PG - 282-7 LID - S0021-9673(15)01019-5 [pii] LID - 10.1016/j.chroma.2015.07.051 [doi] AB - Given the importance of short and medium chain free fatty acids (FFAs) in several fields, this study sought to improve the extraction efficiency of the solid-phase microextraction (SPME) of FFAs by evaluating salting out agents that appear promising for this application. The salts ammonium sulfate ((NH4)2SO4) and sodium dihydrogen phosphate (NaH2PO4) were tried on their own and in combination (3.7/1), in four different total amounts, as salting out agents in the headspace-SPME-gas chromatographic (HS-SPME-GC) analysis of the FFAs from acetic acid (C2) to decanoic acid (C10). Their performance in a model system of an aqueous standard mixture of FFAs at a pH of 3.5 was compared to that of the more commonly used sodium chloride (NaCl) and sodium sulfate (Na2SO4). All of the salts and salt systems evaluated, in proper amount, gave improved results compared to NaCl (saturated), which instead gave interesting results only for the least volatile FFAs C8 and C10. For C2-C6, the salt system that gave the best results compared to NaCl was (NH4)2SO4/NaH2PO4, in the highest of the four amounts evaluated, with factor increases between 1.2 and 4.1-fold, and NaH2PO4, between 1.0 and 4.3-fold. The SPME extraction efficiency given by the mixture (NH4)2SO4/NaH2PO4 was also assessed on biological and food samples, confirming that overall it performed better than NaCl. CI - Copyright (c) 2015 Elsevier B.V. All rights reserved. FAU - Fiorini, Dennis AU - Fiorini D AD - Chemistry Division, School of Science and Technology, University of Camerino, V. S. Agostino 1, I-62032 Camerino, MC, Italy. Electronic address: dennis.fiorini@unicam.it. FAU - Pacetti, Deborah AU - Pacetti D AD - Department of Agricultural, Food, and Environmental Sciences, Universita Politecnica delle Marche, V. Brecce Bianche, I-60131 Ancona, Italy. FAU - Gabbianelli, Rosita AU - Gabbianelli R AD - School of Pharmacy, University of Camerino, V. S. Agostino 1, I-62032 Camerino, MC, Italy. FAU - Gabrielli, Serena AU - Gabrielli S AD - Chemistry Division, School of Science and Technology, University of Camerino, V. S. Agostino 1, I-62032 Camerino, MC, Italy. FAU - Ballini, Roberto AU - Ballini R AD - Chemistry Division, School of Science and Technology, University of Camerino, V. S. Agostino 1, I-62032 Camerino, MC, Italy. LA - eng PT - Journal Article DEP - 20150716 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Acetates) RN - 0 (Decanoic Acids) RN - 0 (Fatty Acids, Nonesterified) RN - 0 (Fatty Acids, Volatile) RN - 0 (Phosphates) RN - 0 (Sulfates) RN - 059QF0KO0R (Water) RN - 0YPR65R21J (sodium sulfate) RN - 451W47IQ8X (Sodium Chloride) RN - 4G9EDB6V73 (decanoic acid) RN - SE337SVY37 (sodium phosphate) RN - SU46BAM238 (Ammonium Sulfate) SB - IM MH - Acetates/analysis MH - Ammonium Sulfate/*chemistry MH - Animals MH - Cheese/analysis MH - Chromatography, Gas/methods MH - Decanoic Acids/analysis MH - Fatty Acids, Nonesterified/*analysis MH - Fatty Acids, Volatile/*analysis MH - Feces/chemistry MH - Gas Chromatography-Mass Spectrometry/methods MH - Phosphates/*chemistry MH - Rats MH - Sodium Chloride/*chemistry MH - Solid Phase Microextraction MH - Sulfates/*chemistry MH - Water MH - Wine/analysis OTO - NOTNLM OT - Ammonium sulfate OT - Free fatty acids OT - Salting out OT - Sodium dihydrogen phosphate OT - Solid-phase microextraction EDAT- 2015/07/27 06:00 MHDA- 2015/12/15 06:00 CRDT- 2015/07/27 06:00 PHST- 2015/06/08 00:00 [received] PHST- 2015/07/10 00:00 [revised] PHST- 2015/07/10 00:00 [accepted] PHST- 2015/07/27 06:00 [entrez] PHST- 2015/07/27 06:00 [pubmed] PHST- 2015/12/15 06:00 [medline] AID - S0021-9673(15)01019-5 [pii] AID - 10.1016/j.chroma.2015.07.051 [doi] PST - ppublish SO - J Chromatogr A. 2015 Aug 28;1409:282-7. doi: 10.1016/j.chroma.2015.07.051. Epub 2015 Jul 16.