Direct separation, identification and quantification of epimers 22R and 22S of budesonide by capillary gas chromatography on a short analytical column with Rtx®-5 stationary phase

Krzek, Jan; Czekaj, Janusz; Rzeszutko, Włodzimierz; Jończyk, Anna

doi:10.1016/j.jchromb.2003.12.038

Cited by 6 publications

(5 citation statements)

References 10 publications

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“…Optimization of the trimethylsilylation by chemometric methods for anabolic agents merits mentioning [107]. However, derivatization is not necessary in all cases: a gas chromatographic alternative without derivatization of the pharmacopoeial HPLC separation of the epimers [8,9] of budesonide is also described [108]. Some further applications of GC to environmental samples are mentioned in Section 5 and Table 2.…”

Section: Other Chromatographic Methodsmentioning

confidence: 99%

Advances in the analysis of steroid hormone drugs in pharmaceuticals and environmental samples (2004–2010)

Gǒrög

2011

Journal of Pharmaceutical and Biomedical Analysis

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Section: Other Chromatographic Methodsmentioning

confidence: 99%

Advances in the analysis of steroid hormone drugs in pharmaceuticals and environmental samples (2004–2010)

Gǒrög

2011

Journal of Pharmaceutical and Biomedical Analysis

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“…Bud is a racemic mixture of two epimers (22 R and 22 S , Figure 1 ). The epimers ratio in the mixture is determined by the synthesis method [ 6 ]. Although they have similar qualitative pharmacological effects, the Bud-22 R is several times more potent than Bud-22 S [ 7 , 8 ].…”

Section: Introductionmentioning

confidence: 99%

“…The identification and quantification of the Bud-22 R and Bud-22 S are carried out by capillary gas chromatography [ 6 ], high performance liquid chromatography (HPLC) [ 9 , 10 ], and sensitive ultra-high-performance liquid chromatography–tandem mass spectrometry method (HPLC-MS) [ 11 , 12 ]. These methods identify Bud epimers indirectly by comparing test samples with reference standards.…”

Section: Introductionmentioning

confidence: 99%

Identification and Quantification by NMR Spectroscopy of the 22R and 22S Epimers in Budesonide Pharmaceutical Forms

et al. 2022

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The authors developed four variants of the qNMR technique (1H or 13C nucleus, DMSO-d6 or CDCl3 solvent) for identification and quantification by NMR of 22R and 22S epimers in budesonide active pharmaceutical ingredient and budesonide drugs (sprays, capsules, tablets). The choice of the qNMR technique version depends on the drug excipients. The correlation of 1H and 13C spectra signals to molecules of different budesonide epimers was carried out on the basis of a comprehensive analysis of experimental spectral NMR data (1H-1H gCOSY, 1H-13C gHSQC, 1H-13C gHMBC, 1H-1H ROESY). This technique makes it possible to identify budesonide epimers and determine their weight ratio directly, without constructing a calibration curve and using any standards. The results of measuring the 22S epimer content by qNMR are comparable with the results of measurements using the reference HPLC method.

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“…To date, a number of techniques have been developed to separate and simultaneously quantify epimers including high performance liquid chromatography (HPLC) 2 , capillary electrophoresis (CE) 3 , capillary gas chromatography 4 , liquid chromatography–mass spectrometry (LC–MS) 5 and liquid chromatography tandem mass spectrometry (LC–MS/MS) 6 . In recent years, assay of epimers has been mainly based on LC–MS/MS which can be considered to involve three-stages of selectivity viz the chromatographic separation, the selection of a precursor ion in quadrupole 1 (Q1) and the selection of one or more product ions in quadrupole 3 (Q3).…”

Section: Introductionmentioning

confidence: 99%

Separation and simultaneous quantitation of PGF2α and its epimer 8-iso-PGF2α using modifier-assisted differential mobility spectrometry tandem mass spectrometry

Liang

Sun

Meng

et al. 2018

Acta Pharmaceutica Sinica B

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Because many therapeutic agents are contaminated by epimeric impurities or form epimers as a result of metabolism, analytical tools capable of determining epimers are increasingly in demand. This article is a proof-of-principle report of a novel DMS–MS/MS method to separate and simultaneously quantify epimers, taking PGF2α and its 8-epimer, 8-iso-PGF2α, as an example. Good accuracy and precision were achieved in the range of 10–500 ng/mL with a run time of only 1.5 min. Isopropanol as organic modifier facilitated a good combination of sensitivity and separation. The method is the first example of the quantitation of epimers without chromatographic separation.

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Direct separation, identification and quantification of epimers 22R and 22S of budesonide by capillary gas chromatography on a short analytical column with Rtx®-5 stationary phase

Cited by 6 publications

References 10 publications

Advances in the analysis of steroid hormone drugs in pharmaceuticals and environmental samples (2004–2010)

Advances in the analysis of steroid hormone drugs in pharmaceuticals and environmental samples (2004–2010)

Identification and Quantification by NMR Spectroscopy of the 22R and 22S Epimers in Budesonide Pharmaceutical Forms

Separation and simultaneous quantitation of PGF2α and its epimer 8-iso-PGF2α using modifier-assisted differential mobility spectrometry tandem mass spectrometry

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