RESUMO
Abstract A stability indicating UPLC method has been developed and validated for the simultaneous determination of fosnetupitant and palonosetron in bulk and in injection dosage form. This combination is used for the prevention of acute and delayed nausea and vomiting associated with initial and repeated courses of highly emetogenic chemotherapy for cancer. The chromatographic analysis was performed on an HSS, RP C18 column (2.1 x 100 mm, 1.8 µm) with an isocratic mobile phase composed of 0.25 M potassium dihydrogen orthophosphate buffer (pH 6.5), pH adjusted with dilute sodium hydroxide:acetonitrile (55:45 v/v), at a flow rate of 0.5 mL/min, and the eluents were monitored at an isosbestic point of 286 nm. The developed method was validated according to the ICH guidelines pertaining to specificity, precision, accuracy, linearity and robustness, and the stability indicating nature of the method was established by forced degradation studies. The retention times of fosnetupitant and palonosetron were observed at 1.390 and 2.404 min, respectively. The developed method proved to be accurate and precise. Linearity was established between 4.70 and 14.10 µg/mL for fosnetupitant and between 0.05 and 0.15 µg/mL for palonosetron. The LOD and LOQ were 0.115 and 0.385 µg/mL, respectively, for fosnetupitant, and 0.005 and 0.016 µg/mL, respectively, for palonosetron. Therefore, the proposed UPLC method was reliable, reproducible, precise and sensitive for the quantification of fosnetupitant and palonosetron.
Assuntos
Estudo de Validação , Palonossetrom/agonistas , Injeções/efeitos adversos , Métodos , Diagnóstico , Formas de Dosagem , Concentração de Íons de Hidrogênio , Neoplasias/prevenção & controleRESUMO
OBJECTIVE:To compare the contents of loganic acid,swertiamarin,6′-O-β-D-glucosyl gentiopicroside,gentiopi-croside,sweroside,isoorientin and isovitexin in wild and cultivated Gentiana officinalis,and to provide basis for rational use of G. officinalis. METHODS:UPLC method was adopted. The separation was performed on ACQUITY UPLC? BEH C18 column (50 mm × 2.1 mm,1.7 μm) with mobile phase consisted of methanol-0.04% phosphoric acid (gradient elution) at the flow rate of 0.3 ml/min. The detection wavelength was set at 242 nm,and column temperature was 30 ℃. RESULTS:For loganic acid,swertiama-rin,6′-O-β- D-glucosyl gentiopicroside,gentiopicroside,sweroside,isoorientin and isovitexin,a good linearity was obtained in the range of 2.1-537.1 μg,1.05-270 μg,0.92-236 μg,11.1-2 830 μg,0.75-192 μg,0.167-102 μg,0.216-52.80 μg(r≥0.999 5), respectively. Their average recoveries were 97.72%-99.84%(RSD≤3.39%,n=6). The contents of loganic acid,swertiamarin, 6′-O-β-D-glucosyl gentiopicroside,gentiopicroside,sweroside and isoorientin in the wild sample were higher than in the cultivat-ed;the content of isovitexin was lower than the cultivated,but there was no statistical significance(P>0.05). The sum of gentiopi-croside and loganin acid content were all higher than 2.5% in both wild and cultivated samples,and met the requirements of 2015 edition of Chinese Pharmacopoeia(first part). CONCLUSIONS:The content difference of 7 indicative constituents in wild and cul-tivated G. officinalis is not statistically significant,and the indicative constituents of the pharmacopoeia is qualified.
RESUMO
OBJECTIVE: To establish an UPLC method for the determination of eleven flavonoid glycosides in Ginkgo biloba extract. METHODS: The analysis was performed on an Agilent ZORBAX Eclipse Plus C18 column(4.6 mm × 50 mm, 1.8 μm). Mobile phase A was acetonitrile, mobile phase B was 0.4% phosphoric acid, and gradient elution was carried out at a flow rate of 0.6 mL · min-1. The detection was carried out at 360 nm. RESULTS: The calibration curves of the eleven flavonoid glycosides had good linearinities with good recoveries. CONCLUSION: The method is simple, rapid, accurate, reliable, high sensitive, and can be used as the quantity control method of Ginkgo biloba extract.