Silica hydride based phases for small molecule separations using automated liquid chromatography–mass spectrometry method development

Appulage, Dananjaya K.; Schug, Kevin A.

doi:10.1016/j.chroma.2017.05.073

Cited by 7 publications

(12 citation statements)

References 26 publications

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“…A model sample mixture was used during method development for simultaneous analysis of small molecules and proteins. The small molecules were selected from various analyte classes with different functional groups so that they exhibit different retention behaviors (Supporting Information Figure S1) . In the case of proteins, inexpensive, widely available, and commonly used protein standards were used.…”

Section: Resultsmentioning

confidence: 99%

“…According to the literature, it was shown that more hydrophilic analytes require more hydrophobic phases, such as C8 or C18, to be retained . In most applications, RAM columns have been used to concentrate or trap small molecules and separate them from protein interferences . In those cases, the small molecules were hydrophobic enough to be trapped, and the wash effluent from the trap column was simply directed to waste.…”

Section: Resultsmentioning

confidence: 99%

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An integrated multipath liquid chromatography–mass spectrometry system for the simultaneous preparation, separation, and detection of proteins and small molecules

Appulage

Wang

Figard³

et al. 2018

J of Separation Science

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A multipath liquid chromatography with mass spectrometry instrument was constructed with the help of restricted access media to online segregate small and large molecules. This liquid chromatography system was custom built with five pumps and three two-position six-port valves to control the flow in a multipath system for the simultaneous analysis of small molecules and proteins. On separate chromatographic channels, small molecules trapped and proteins excluded from the online restricted access media were analyzed downstream using high-efficiency columns and a triple quadrupole mass spectrometer. A model sample, which included five proteins and 22 small molecules with different physicochemical properties, was used to evaluate the system. Following injection, the complete multipath separation and detection was performed in 22 min. Protein exclusion by the restricted access media was not quantitative. Four commercial trap columns were evaluated for their exclusion efficiency toward the proteins. Exclusion efficiency varied from <50% to only a maximum of 75% exclusion across the trap columns tested. An attempt was made to optimize the exclusion efficiency using different flow rates, flow rate gradients, and different additives both in the sample and the mobile phases. Protein exclusion was still erratic and generally nonquantitative.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

An integrated multipath liquid chromatography–mass spectrometry system for the simultaneous preparation, separation, and detection of proteins and small molecules

Appulage

Wang

Figard³

et al. 2018

J of Separation Science

Self Cite

View full text Add to dashboard Cite

show abstract

“…173 To find the most appropriate stationary phase and mobile phase conditions, it might be useful to initially perform a screening process (often known as "scouting"), as prior knowledge influences the choices. 164,[174][175][176] Screening is typically performed on three or four selected columns possessing different chemistries and operating at three different mobile phase pH values in addition to using two different organic modifiers and performing a generic (short) gradient. Then, the number of resolved peaks, peak shapes and elution windows are usually compared to determine the best combination of stationary phase and mobile phase.…”

Section: Automated Tools For Methods Development In Chromatographymentioning

confidence: 99%

Recent Advances in Chromatography for Pharmaceutical Analysis

et al. 2018

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“…To further improve LC separations and sample analysis, silica hydride (SiH) stationary phases have recently been explored for small molecules and emerging drugs of abuse [20][21][22][23] including the separation of two synthetic cathinone m/z 177 positional isomers [21]. Stationary phases exhibiting a "U-shaped" retention curve with varying percent organic are operable under both RPC and HILIC/aqueous normal phase (ANP) modes.…”

Section: Introductionmentioning

confidence: 99%

“…Stationary phases exhibiting a "U-shaped" retention curve with varying percent organic are operable under both RPC and HILIC/aqueous normal phase (ANP) modes. They include both the SiH phases [23] and the classical silica pentaflurophenyl (PFP) phase [24][25]. Operation of a column under two modes using the same solvent reservoir has been coined as "flipflop" chromatography [25].…”

Section: Introductionmentioning

confidence: 99%

The utility of silica hydride‐based stationary phases for dual‐mode ultra high performance liquid chromatography separation of synthetic cathinone positional isomers

Ploumen

Marginean

Lurie

2020

J of Separation Science

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Emerging drugs usually mimic the effects of traditional drugs, but are not always controlled due to the chemically altered structures. Positional isomers of emerging drugs are difficult to analyze because they challenge the separation and detection techniques commonly employed by forensic laboratories. The utility of silica hydride stationary phases for the ultra‐high performance liquid chromatography separation of synthetic cathinone positional isomers was studied in this manuscript. SiH phases are operable under both reversed phase and aqueous normal phase chromatographic conditions without the need to change solvent reservoirs. The separation of eight positional isomers of the synthetic cathinone, pentedrone, was investigated using five silica hydride phases, and compared to a classical dual column reversed phase, hydrophilic interaction chromatography system, and to a bimodal pentaflurophenyl column. Significant selectivity differences were observed using either a combination of a classical reversed phase C18 and NP Silica columns or the various bimodal columns. The silica hydride silica‐C column, which contains no derivatized ligands attached to the silica hydride backbone, not only gave the most orthogonal separation of the bimodal columns, but provided a unique separation of all eight positional isomers (resolution ≥ 1) using the combination of reverse phase and aqueous normal phase chromatographic conditions.

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Silica hydride based phases for small molecule separations using automated liquid chromatography–mass spectrometry method development

Cited by 7 publications

References 26 publications

An integrated multipath liquid chromatography–mass spectrometry system for the simultaneous preparation, separation, and detection of proteins and small molecules

An integrated multipath liquid chromatography–mass spectrometry system for the simultaneous preparation, separation, and detection of proteins and small molecules

Recent Advances in Chromatography for Pharmaceutical Analysis

The utility of silica hydride‐based stationary phases for dual‐mode ultra high performance liquid chromatography separation of synthetic cathinone positional isomers

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