A simple, accurate, rapid and sensitive reversed-phase high-performance liquid chromatography (RP-HPLC) method was established for determination of a novel non-vitamin K antagonist oral anticoagulant drug, betrixaban, and its co-administered calcium-channel blocker drug, lercanidipine, in pharmaceutical formulations and biological fluids. The proposed HPLC method was the first chromatographic method applied to estimate this mixture in a short chromatographic run (<6 min), high resolution between betrixaban/lercanidipine (Rs = 7.12) and acceptable values of limit of detection (LOD), limit of quantification (LOQ) and percentage of relative standard deviation (%RSD). The chromatographic separation was performed on a cyano column using a mobile phase composed of acetonitrile:methanol:water (35:35:30, v/v/v) containing 0.2% orthophosphoric acid adjusted to pH 3.2 by triethylamine, programmed with a flow rate of 1 mL/min with UV detection at 240 nm. The proposed method showed linearity over the concentration ranges of (0.20–20.0 μg/mL) and (0.25–25.0 μg/mL) for betrixaban and lercanidipine, respectively. All validation parameters met the acceptance criteria according to ICH guidelines in terms of linearity, LOD, LOQ, accuracy, precision, robustness, specificity and system suitability. The method was applied to assay the studied analytes in their pharmaceutical formulations with high % recovery (98–102%) and low %RSD (<1.5). Furthermore, the proposed method was successfully applied for the determination of betrixaban in spiked human plasma.
Background:The first highly sensitive, rapid and specific green microemulsion liquid
chromatographic (MELC) method was established for the simultaneous estimation of fluticasone propionate
(FLU) and azelastine HCl (AZL) in the presence of their pharmaceutical dosage form additives
(phenylethyl alcohol (PEA) and benzalkonium chloride (BNZ)).Methods:The separation was performed on a C18 column using (o/w) microemulsion as a mobile
phase which contains 0.2 M sodium dodecyl sulphate (SDS) as surfactant, 10% butanol as cosurfactant,
1% n-octanol as internal phase and 0.3% triethylamine (TEA) adjusted at pH 6 by 0.02 M
phosphoric acid; with UV detection at 220 nm and programmed with flow rate of 1 mL/min.Results:The validation characteristics e.g. linearity, lower limit of quantification (LOQ), lower limit
of detection (LOD), accuracy, precision, robustness and specificity were investigated. The proposed
method showed linearity over the concentration range of (0.5-25 µg/mL) and (0.1-25 µg/mL) for FLU
and AZL, respectively. Besides that, the method was adopted in a short chromatographic run with satisfactory
resolution factors of (2.39, 3.78 and 6.74 between PEA/FLU, FLU/AZL and AZL/BNZ), respectively.
The performed method was efficiently applied to pharmaceutical nasal spray with (mean
recoveries ± SD) (99.80 ± 0.97) and (100.26 ± 0.96) for FLU and AZL, respectively.Conclusion:The suggested method was based on simultaneous determination of FLU and AZL in the
presence of PEA and BNZ in pure form, laboratory synthetic mixture and its combined pharmaceutical
dosage form using green MELC technique with UV detection. The proposed method appeared to
be superior to the reported ones of being more sensitive and specific, as well as the separation was
achieved with good performance in a relatively short analysis time (less than 7.5 min). Highly acceptable
values of LOD and % RSD make this method superior to be used in quality control laboratories
with of HPLC technique.
Green solvents such as microemulsion were used in the proposed method because they play a vital role in the analytical method's influence on the environment. A highly sensitive, specific, and validated stability-indicating eco-friendly green microemulsion liquid chromatography (MELC) method was developed for separation of the antihistaminic drug Azelastine HCl (AZL) from its degradation products with application to degradation kinetics. Chromatographic separation was operated on a C column with a microemulsion mobile phase, which consists of 0.1 M sodium dodecyl sulphate, 10% -propanol, 1%-octanol, and 0.3% triethylamine, by using 0.02 M phosphoric acid at pH 3.5 and irbesartan as internal standard. The eluted compounds were monitored at 210 nm with flow rate 1 mL/min at ambient temperature. A linear dependence of the peak area on drug concentration over the concentration range of 0.1 to 25 μg/mL was achieved with an LOD of 0.04 μg/mL and an LOQ of 0.10 μg/mL. Moreover, the proposed method was successfully applied for determination of AZL in eye drops and metered dose nasal inhaler as well as to study the kinetics of alkaline, acidic, neutral, oxidative, and photolytic degradation processes of AZL according to the International Council for Harmonization guidelines. The proposed method could be used as a harmless alternative for quality control analysis of the mentioned drug, without interference from dosage form additives or decomposition products. A highly sensitive stability-indicating eco-friendly green MELC method was developed for the separation of the antihistaminic drug AZL from its degradation products.
A facile, rapid, accurate and selective quantitative proton nuclear magnetic resonance (
1
H-qNMR) method was developed for the simultaneous determination of fluticasone propionate (FLP) and azelastine hydrochloride (AZH) in pharmaceutical nasal spray for the first time. The
1
H-qNMR analysis of the studied analytes was performed using inositol as the internal standard and dimethyl sulfoxide-
d
6
(DMSO-
d
6
)
as the solvent. The quantitative selective proton signal of FLP was doublet of doublet at 6.290, 6.294, 6.316 and 6.319 ppm, while that of AZH was doublet at 8.292 and 8.310 ppm. The internal standard (inositol) produced a doublet signal at 3.70 and 3.71 ppm. The method was rectilinear over the concentration ranges of 0.25–20.0 and 0.2–15.0 mg ml
−1
for FLP and AZH, respectively. No labelling or pretreatment steps were required for NMR analysis of the studied analytes. The proposed
1
H-qNMR method was validated efficiently according to the International Council on Harmonisation guidelines in terms of linearity, limit of detection, limit of quantification, accuracy, precision, specificity and stability. Moreover, the method was applied to assay the analytes in their combined nasal spray formulation. The results ensured the linearity (
r
2
> 0.999), precision (% RSD < 1.5), stability, specificity and selectivity of the developed method.
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