Flame-induced atmospheric pressure chemical ionization (FAPCI) has been used to directly characterize chemical compounds on a glass rod and drug tablet surfaces. In this study, FAPCI was further applied to interface thin layer chromatography (TLC) and mass spectrometry (MS) for mixture analysis.Methods: A micro-sized oxyacetylene flame was generated using a small concentric tube system. Hot gas flow and primary reactive species from the micro-flame were directed toward a developed TLC gel plate to thermally desorb and ionize analytes on the gel surface. The resulting analyte ions subsequently entered the MS inlet for detection.Results: A 1-1.5-mm-wide light-brown line was observed on the TLC plate after the desorption FAPCI/MS (DFAPCI/MS) analysis, revealing that the gel surface withstood a high temperature from the impact of the micro-flame. Volatile and semivolatile chemical compounds, including amine and amide standards, drugs, and aromatherapy oils, were successfully desorbed, ionized, and detected using this TLC/DFAPCI/MS. The limit of detection of TLC-DFAPCI/MS was determined to be 5 ng/spot for dibenzylamine and ethenzamide.Conclusions: TLC/DFAPCI/MS is one of the simplest TLC-MS interfaces showing the advantages such as low costs and an easy set up. The technique is useful for characterizing thermally stable volatile and semi-volatile compounds in a mixture.
Rationale
Thermogravimetry (TG) combined with electrospray and atmospheric chemical ionization (ESI+APCI) mass spectrometry (MS) was developed to rapidly characterize thermal decomposition products of synthetic polymers and plastic products. The ESI‐based TG‐MS method is useful for characterizing thermally labile, nonvolatile, and polar compounds over an extensive mass range; and the APCI‐based TG‐MS counterpart is useful for characterizing volatile and nonpolar compounds. Both polar and nonpolar compounds can be simultaneously detected by ESI+APCI‐based TG–MS.
Methods
Analytes with different volatility were produced from TG operated at different temperatures, which were delivered through a heated stainless‐steel tube to the ESI+APCI source where they reacted with the primary charged species generated from electrospray and atmospheric pressure chemical ionization (ESI+APCI) of solvent and nitrogen. The analyte ions were then detected by an ion trap mass spectrometer.
Results
A semi‐volatile PEG 600 standard was used as the sample and protonated and sodiated molecular ions together with adduct ions including [(PEG)n + 15]+, [(PEG)n + 18]+, and [(PEG)n + 29]+ were detected by TG‐ESI+APCI‐MS. The technique was further utilized to characterize thermal decomposition products of nonvolatile polypropylene glycol (PPG) and polystyrene (PS) standards, as well as a PS‐made water cup and coffee cup lid. The characteristic fragments of PPG and PS with mass differences of 58 and 104 between respective ion peaks were detected at the maximum decomposition temperature (Tmax).
Conclusions
The information obtained from the TG–ESI+APCI‐MS analysis is useful in rapidly distinguishing different types of polymers and their products. In addition, the signals of the additives in the polymer products, including antioxidants and plasticizers, were also detected before the TG temperature reached Tmax.
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