PMID- 22881719 OWN - NLM STAT- MEDLINE DCOM- 20130111 LR - 20131121 IS - 1520-6882 (Electronic) IS - 0003-2700 (Linking) VI - 84 IP - 17 DP - 2012 Sep 4 TI - Quantitative real-time monitoring of chemical reactions by autosampling flow injection analysis coupled with atmospheric pressure chemical ionization mass spectrometry. PG - 7547-54 LID - 10.1021/ac3017136 [doi] AB - Although qualitative and/or semiquantitative real-time monitoring of chemical reactions have been reported with a few mass spectrometric approaches, to our knowledge, no quantitative mass spectrometric approach has been reported so far to have a calibration valid up to molar concentrations as required by process control. This is mostly due to the absence of a practical solution that could well address the sample overloading issue. In this study, a novel autosampling flow injection analysis coupled with an atmospheric pressure chemical ionization mass spectrometry (FIA/APCI-MS) system, consisting of a 1 muL automatic internal sample injector, a postinjection splitter with 1:10 splitting ratio, and a detached APCI source connected to the mass spectrometer using a 4.5 in. long, 0.042 in. inner diameter (ID) stainless-steel capillary, was thus introduced. Using this system together with an optional FIA solvent modifier, e.g., 0.05% (v/v) isopropylamine, a linear quantitative calibration up to molar concentration has been achieved with 3.4-7.2% relative standard deviations (RSDs) for 4 replicates. As a result, quantitative real-time monitoring of a model reaction was successfully performed at the 1.63 M level. It is expected that this novel autosampling FIA/APCI-MS system can be used in quantitative real-time monitoring of a wide range of reactions under diverse reaction conditions. FAU - Zhu, Zhenqian AU - Zhu Z AD - Mass Spectrometry Center, Department of Chemistry, University of Tennessee, Knoxville, Tennessee 37996-1600, United States. FAU - Bartmess, John E AU - Bartmess JE FAU - McNally, Mary Ellen AU - McNally ME FAU - Hoffman, Ron M AU - Hoffman RM FAU - Cook, Kelsey D AU - Cook KD FAU - Song, Liguo AU - Song L LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PT - Research Support, U.S. Gov't, Non-P.H.S. DEP - 20120821 PL - United States TA - Anal Chem JT - Analytical chemistry JID - 0370536 RN - 0 (Phenethylamines) RN - 0 (Propylamines) RN - 0 (Solvents) RN - 327C7L2BXQ (phenethylamine) RN - MP1U0D42PE (Acrylonitrile) RN - P8W26T4MTD (2-propylamine) SB - IM MH - Acrylonitrile/chemistry MH - Atmospheric Pressure MH - Automation MH - Calibration MH - Flow Injection Analysis MH - Phenethylamines/analysis MH - Propylamines/chemistry MH - Solvents/chemistry MH - Spectrometry, Mass, Electrospray Ionization/instrumentation/*methods/standards EDAT- 2012/08/14 06:00 MHDA- 2013/01/12 06:00 CRDT- 2012/08/14 06:00 PHST- 2012/08/14 06:00 [entrez] PHST- 2012/08/14 06:00 [pubmed] PHST- 2013/01/12 06:00 [medline] AID - 10.1021/ac3017136 [doi] PST - ppublish SO - Anal Chem. 2012 Sep 4;84(17):7547-54. doi: 10.1021/ac3017136. Epub 2012 Aug 21.