Search for improved fluorinated stationary phases for separation of fluorine-containing pharmaceuticals from their desfluoro analogs

Regalado, Erik L.; Makarov, Alexey A.; McClain, Ray T.; Przybyciel, Matthew; Welch, Christopher J.

doi:10.1016/j.chroma.2014.12.025

Cited by 31 publications

(10 citation statements)

References 17 publications

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“…These phases have often been cited as having "U-shaped" retention behavior similar to that which has been reported on silica hydride. As expected, phases made from traditional organosilanization display significant reversed-phase behavior and also some selectivity for fluorinated analytes [18]. However, as shown in Fig.…”

Section: Comparison To Other Fluorinated Phasesmentioning

confidence: 81%

Evaluation of the dual retention properties of stationary phases based on silica hydride: Perfluorinated bonded material

Pesek

Matyska

Natekar

2016

J of Separation Science

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The synthesis of a new perfluorinated stationary phase based on silica hydride using a hydrosilation reaction was investigated. The material was characterized by elemental analysis, diffuse reflectance infrared Fourier transform spectroscopy and (13) C cross-polarization magic-angle spinning NMR spectroscopy. The retention properties of this new material were tested in the reversed-phase and normal-phase mode. Variable buffer strength experiments at two pH conditions for selected polar compounds were used to compare the new phase to hydrophilic interaction liquid chromatography retention. These results and previous data reported in the literature were used to postulate differences in the retention mechanism between hydrophilic interaction liquid chromatography and silica hydride-based stationary phases.

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Section: Comparison To Other Fluorinated Phasesmentioning

confidence: 81%

Evaluation of the dual retention properties of stationary phases based on silica hydride: Perfluorinated bonded material

Pesek

Matyska

Natekar

2016

J of Separation Science

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“…Both compounds' pKa values are lower than the pH of the eluent and being basic compounds they are deprotonated (neutral), explaining longer retention times than those of glucuronides. The fluorinated stationary phase provides alternate selectivity for the fluorinated analytes [29] midazolam and MiOH. Besides having a similar structure to midazolam, MiOH is more polar and it elutes faster.…”

Section: Methods Development and The Chromatographic Retentionmentioning

confidence: 99%

A highly sensitive method for the simultaneous UHPLC–MS/MS analysis of clonidine, morphine, midazolam and their metabolites in blood plasma using HFIP as the eluent additive

Veigure

Aro

Metsvaht

et al. 2017

Journal of Chromatography B

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In intensive care units, the precise administration of sedatives and analgesics is crucial in order to avoid under- or over sedation and for appropriate pain control. Both can be harmful to the patient, causing side effects or pain and suffering. This is especially important in the case of pediatric patients, and dose-response relationships require studies using pharmacokinetic-pharmacodynamic modeling. The aim of this work was to develop and validate a rapid ultra-high performance liquid chromatographic-tandem mass spectrometric method for the analysis of three common sedative and analgesic agents: morphine, clonidine and midazolam, and their metabolites (morphine-3-glucuronide, morphine-6-glucuronide and 1'-hydroxymidazolam) in blood plasma at trace level concentrations. Low concentrations and low sampling volumes may be expected in pediatric patients; we report the lowest limit of quantification for all analytes as 0.05ng/mL using only 100μL of blood plasma. The analytes were separated chromatographically using the C18 column with the weak ion-pairing additive 1,1,1,3,3,3-hexafluoro-2-propanol and methanol. The method was fully validated and a matrix matched calibration range of 0.05-250ng/mL was attained for all analytes In addition, between-day accuracy for all analytes remained within 93-108%, and precision remained within 1.5-9.6% for all analytes at all concentration levels over the calibration range.

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“…In an in-depth study of this phenomenon, we found that specialized halogenated stationary phases were often effective for resolution of such mixtures. [103][104][105] In addition, the excellent shape-selectivity of chiral stationary phases makes them well suited for dealing with many challenging separations of closely related species. 106,107 Interestingly, a study of the separation problems of academia showed that many academic separation challenges involve the resolution of closely related species, which can often be addressed using modern separation science tools from the pharmaceutical industry.…”

Section: Analysis Of Closely Related Speciesmentioning

confidence: 99%

High throughput analysis enables high throughput experimentation in pharmaceutical process research

Welch

2019

React. Chem. Eng.

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Search for improved fluorinated stationary phases for separation of fluorine-containing pharmaceuticals from their desfluoro analogs

Cited by 31 publications

References 17 publications

Evaluation of the dual retention properties of stationary phases based on silica hydride: Perfluorinated bonded material

Evaluation of the dual retention properties of stationary phases based on silica hydride: Perfluorinated bonded material

A highly sensitive method for the simultaneous UHPLC–MS/MS analysis of clonidine, morphine, midazolam and their metabolites in blood plasma using HFIP as the eluent additive

High throughput analysis enables high throughput experimentation in pharmaceutical process research

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