PMID- 33838765 OWN - NLM STAT- PubMed-not-MEDLINE DCOM- 20210419 LR - 20210419 IS - 1873-3573 (Electronic) IS - 0039-9140 (Linking) VI - 229 DP - 2021 Jul 1 TI - Simultaneous determination of short-chain fatty alcohols in aged oil and biodiesels by stable isotope labeling assisted liquid chromatography-mass spectrometry. PG - 122223 LID - S0039-9140(21)00144-2 [pii] LID - 10.1016/j.talanta.2021.122223 [doi] AB - Short-chain fatty alcohols (SCFAs) are one of the reactants for the production of biodiesels. The SCFA residues at the trace level have a significant impact on biodiesel quality. However, the analysis of SCFAs in aged biodiesels has not been reported so far, which is probably due to the unavailability of an appropriate analytical method for the simultaneous determination of SCFAs. Herein, we developed a novel analytical approach with high sensitivity and selectivity for the simultaneous identification and determination of SCFAs in seed oil and biodiesel samples during the simulated real-time aging by stable isotope labeling assisted liquid chromatography-mass spectrometry (SIL-LC-MS). A pair of isotope labeling reagents, pyridine (Py) and [(2)H(5)]pyridine ([(2)H(5)]Py), were used to label SCFAs in biodiesels and standards, respectively. The [(2)H(5)]Py labeled SCFAs were used as internal standards to compensate for the detection of variances. The simultaneous determination of SCFAs was performed by LC-MS with an improved detection selectivity and sensitivity. The limits of detection (LODs) values were ranged from 0.2 to 0.5 ng mL(-1) for the investigated SCFAs. Good linearity was observed in the studied ranges (R(2) > 0.99) and good precision with relative standard deviations (RSDs) was in the range of 4.9-18.1%. Average recoveries were obtained in the range of 80.3%-115.4%. The matrix effects were in the range of 70.0-104.3%. The validated SIL-LC-MS method was applied to the simultaneous quantitative analysis of SCFAs in seed oil and biodiesel samples and the LC-MS analysis could be done within 3 min. The formation mechanism of SCFAs in aged oil and biodiesel samples was also investigated by this method. The results suggest that SCFAs were formed and their composition changed during the simulated real-time aging of long-chain fatty acid (LCFA), long-chain fatty acid methyl ester (FAME), seed oil, and biodiesels. Moreover, we found that the formation of 1-pentanol and 1-hexanol was associated with the number and position of double bonds in LCFAs and FAMEs. CI - Copyright (c) 2021 Elsevier B.V. All rights reserved. FAU - Xiao, Hua-Ming AU - Xiao HM AD - Key Laboratory of Analytical Chemistry of the State Ethnic Affairs Commission, College of Chemistry and Materials Science, South-Central University for Nationalities, Wuhan, 430074, People's Republic of China. FAU - Zhao, Shuai AU - Zhao S AD - School of Pharmaceutical Engineering &; Life Science, Changzhou University, Changzhou, 213164, People's Republic of China. FAU - Fan, Ru-Ting AU - Fan RT AD - Key Laboratory of Analytical Chemistry of the State Ethnic Affairs Commission, College of Chemistry and Materials Science, South-Central University for Nationalities, Wuhan, 430074, People's Republic of China. FAU - Hussain, Dilshad AU - Hussain D AD - HEJ Research Institute of Chemistry, International Center for Chemical and Biological Sciences, University of Karachi, Karachi, 75270, Pakistan. FAU - Wang, Xian AU - Wang X AD - Key Laboratory of Analytical Chemistry of the State Ethnic Affairs Commission, College of Chemistry and Materials Science, South-Central University for Nationalities, Wuhan, 430074, People's Republic of China. Electronic address: xwang27@mail.scuec.edu.cn. LA - eng PT - Journal Article DEP - 20210309 PL - Netherlands TA - Talanta JT - Talanta JID - 2984816R SB - IM OTO - NOTNLM OT - Biodiesel OT - Liquid chromatography-tandem mass spectrometry OT - Seed oil OT - Short-chain fatty alcohols (SCFAs) OT - Stable isotope labeling EDAT- 2021/04/12 06:00 MHDA- 2021/04/12 06:01 CRDT- 2021/04/11 20:19 PHST- 2020/12/16 00:00 [received] PHST- 2021/02/03 00:00 [revised] PHST- 2021/02/13 00:00 [accepted] PHST- 2021/04/11 20:19 [entrez] PHST- 2021/04/12 06:00 [pubmed] PHST- 2021/04/12 06:01 [medline] AID - S0039-9140(21)00144-2 [pii] AID - 10.1016/j.talanta.2021.122223 [doi] PST - ppublish SO - Talanta. 2021 Jul 1;229:122223. doi: 10.1016/j.talanta.2021.122223. Epub 2021 Mar 9.