Development and validation of GLC/MS-procedure of doxylamine quantitative determination
Journal Title: Журнал органічної та фармацевтичної хімії; Журнал органической и фармацевтической химии - Year 2019, Vol 17, Issue 2
Abstract
Doxylamine is a hypnotic medicine used for treatment of minor sleep disorders and is a frequent cause of poisoning. Aim. To develop GLC/MS-procedure of doxylamine quantification and carry out step-by-step validation of the developed procedure in the variants of the method of calibration curve, method of standard and method of additions. Results. The chromatographic conditions have been chosen for doxylamine determination by the method of GLC with mass-spectrometry detection with temperature program changing during the analysis from 70 °C to 320 °C. Retention time for doxylamine is 14.53 min. To prove the possibility of the proposed procedure application in further analysis its validation has been carried out in the variants of the method of calibration curve, method of standard and method of additions. Such validation parameters as in process stability, linearity, accuracy, precision and limit of determination have been estimated by model solutions. Experimental part. Conditions of chromatographic analysis: Agilent 6890N/5973N/7683; НР-5MS 0.25 mm × 30 m, 0.25 μm; DB-17MS 0.25 mm × 30 m, 0.15 μm; columns are connected sequentially through Deans switch; thermostat – 70 ºС (2 min), 45 ºС/min to 210 ºС, 6 ºС/min to 320 ºС (12.56 min); transfer line – 280 ºС; ion source – 230 ºС; quadrupole – 150 ºС; electron impact, 70eV; 40 – 750 m/z; injector – 250 ºС; splitless mode; inlet carrier gas (helium) pressure: 1st column – 26.06 psi, 2nd column – 19.30 psi. Conclusions. New procedure of doxylamine quantitative determination by the method of GLC/MS has been developed. Its validation has been carried out and acceptability for application has been shown.
Authors and Affiliations
L. Yu. Klimenko, S. M. Trut, Т. A. Kostina
Keywords
Related Articles
- EP ID EP658511
- DOI 10.24959/ophcj.19.974
- Views 57
- Downloads 0
Квантово-хімічне дослідження механізму реакції епоксидування гераніолу та лимонену надацетатною та надбензойною кислотами
Мета – з’ясування механізму реакції епоксидування терпеноїдів Гераніолу та Лимонену надацетатною (пероксіетановою) та надбензойною кислотами за результатами квантово-хімічного дослідження. Матеріали та методи. Для розра...
The synthesis of polisubstituted thienylpyrroles and the study of their activity as plant growth stimulators
Aim. To develop the optimal method for the synthesis of new polysubstituted thienylpyrroles and study them as cereal growth stimulants. Results and discussion. Preparative methods for the synthesis of 4-(5-carboxythiophe...
The acid-base properties of 2-(benzoylamino)(1-R-2-oxoindolin-3-ylidene)acetic acids
Aim. To study the acid-base properties of derivatives of 2-(benzoylamino)(1-R-2-oxoindolin-3-ylidene)acetic acid substituted by the location 1 of oxoindolin fragment. Results and discussion. The compounds studied are wea...
Development and validation of the enzymatic kinetic photometric procedure for determination of residual quantities of dequalinium chloride on the surface of the pharmaceutical equipment
Aim. To develop and validate the new enzymatic kinetic photometric procedure for analysis of dequalinium chloride based on application of enzymatic acetylcholine hydrolysis to determine the residual quantities of dequali...
Synthesis and antioxidant properties of novel thiazolo[4,5-b]pyridine-2-ones
Aim. To expand the synthetic potential of thiazolo[4,5-b]pyridines, study the reactivity and perform the pharmacological screening of the antioxidant activity of the novel compounds synthesized. Results and discussion. A...