Guidelines for successful SFC/MS

Pinkston, J. David; Chester, T. L.

doi:10.1021/ac00117a001

Cited by 18 publications

(13 citation statements)

References 17 publications

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“…Several mass spectrometric techniques have been used for characterization of silicone oils, either alone or in combination with separation techniques, e.g. GC–MS,6, 7 on‐line SFC‐MS,8–10 off‐line SFC‐MS,11 size exclusion chromatography (SEC),12, 13 high‐performance LC (HPLC)14 and SFC15 in combination with matrix‐assisted laser desorption ionization–time‐of‐flight MS (MALDI–TOF MS).…”

Section: Introductionmentioning

confidence: 99%

Determination of molecular mass distribution of silicone oils by supercritical fluid chromatography, matrix‐assisted laser desorption ionization time‐of‐flight mass spectrometry and their off‐line combination

2001

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Silicone oil samples were characterized by supercritical fluid chromatography (SFC), matrix-assisted laser desorption ionization-time-of-flight mass spectrometry (MALDI--TOF MS), and their off-line combination. SFC was used to separate samples of silicone oils on micropacked capillary columns. The fractions for the identification studies were obtained from SFC runs at defined time intervals, when the restrictor was pulled out from the chromatographic flame ionization detector (FID) and inserted into a glass vial with acetone. MALDI--TOF MS was used for the identification of individual oligomers in the fractions separated. The molecular mass distributions determined based on SFC and MALDI--TOF MS measurements were compared. From this comparison, it follows that the results are in good agreement. However, certain differences were observed: MALDI--TOF MS was capable of detecting somewhat larger oligomers than the SFC-FID, but the lower molecular mass oligomers were not present in the MALDI spectra. Differences in the region of lower molecular masses can be explained by evaporation of the more volatile low molecular mass oligomers resulting from heating of the sample during the MALDI--TOF MS measurements as a result of the absorption of the laser shot energy. The fact that no high mass discrimination effects of the MALDI--TOF MS measurements, compared with SFC, were observed is very promising for further applications of MALDI--TOF MS in characterizing synthetic polymers of moderate polydispersity.

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Section: Introductionmentioning

confidence: 99%

Determination of molecular mass distribution of silicone oils by supercritical fluid chromatography, matrix‐assisted laser desorption ionization time‐of‐flight mass spectrometry and their off‐line combination

2001

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“…The use of SFC should expand as knowledge of its advantages accumulates, especially in high-throughput applications. , Since it is often of interest to separate multicomponent mixtures in a minimal amount of time, the technique is finding increased use in industry for applications in which liquid chromatography separations are considered too slow. Similarly, when mass analysis of the analytes is necessary, SFC/MS will begin to replace LC/MS. − …”

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confidence: 99%

Packed Column Supercritical Fluid Chromatography/Mass Spectrometry for High-Throughput Analysis

et al. 1999

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A supercritical fluid chromatograph was interfaced to a mass spectrometer, and the system was evaluated for applications requiring high sample throughput. Experiments presented demonstrate the high-speed separation capability of supercritical fluid chromatography (SFC) and the effectiveness of supercritical fluid chromatography/mass spectrometry (SFC/MS) for fast, accurate determinations of multicomponent mixtures. A high-throughput liquid chromatography/mass spectrometry (LC/MS) analysis cycle time is reduced 3-fold using our general SFC/MS high-throughput method, resulting in substantial time saving for large numbers of samples. Unknown mixture characterization is improved due to the increased selectivity of SFC/MS compared to LC/MS. This was demonstrated with sample mixtures from a 96-well combinatorial library plate. In this paper, we report a negative mode atmospheric pressure chemical ionization (APCI) method for SFC/MS suitable for most of the components in library production mixtures. Flow injection analysis (FIA) also benefits from this SFC/MS system. A broader range of solvents is amenable to the SFC mobile phase compared with standard LC/MS solvents, and solutes elute more rapidly from the SFC/MS system, reducing sample carryover and cycle time. Finally, our instrumental setup allows for facile conversion between LC/MS and SFC/MS modes of operation.

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“…For applications published before the year 2000, several reviews can be of comprehensive use to readers [34][35][36][37]. For applications published before the year 2000, several reviews can be of comprehensive use to readers [34][35][36][37].…”

Section: Chiral Sfc On Drug Compounds and Intermediatesmentioning

confidence: 99%

Separations of Chiral Compounds by SFC

Wang

2010

Chiral Separation Methods for Pharmaceutical and Biotechnological Products

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Guidelines for successful SFC/MS

Cited by 18 publications

References 17 publications

Determination of molecular mass distribution of silicone oils by supercritical fluid chromatography, matrix‐assisted laser desorption ionization time‐of‐flight mass spectrometry and their off‐line combination

Determination of molecular mass distribution of silicone oils by supercritical fluid chromatography, matrix‐assisted laser desorption ionization time‐of‐flight mass spectrometry and their off‐line combination

Packed Column Supercritical Fluid Chromatography/Mass Spectrometry for High-Throughput Analysis

Separations of Chiral Compounds by SFC

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