Development and validation of a new and economical stability indicating RP-HPLC method for cefixime trihydrate

ABSTRACT The present work describes the development of a new high performance liquid chromatographic (HPLC) method for the determination of Cefixime trihydrate under different stress conditons as specified by ICH. For the analysis, a Phenomenex (250 x 4.6 mm, 5 µm particle size) ODS column and a SPD 20 A UV detector at 289 nm was used. The selected mobile phase was 10 mM disodium hydrogen phosphate (with 0.5% TEA, pH adjusted to 6.3 with OPA) and methanol in the ratio of 75:25 (v/v) in isocratic mode at a flow rate of 1 mL.min-1.The linear regression analysis data for the calibration plots showed good linear relationship with r2 = 0.9997 in the concentration range of 5-100 μg.mL-1. The stress degradation was performed using acid, alkali, water, hydrogen peroxide and uv light.

RESUMO O presente trabalho descreve o desenvolvimento de um novo alta performance cromatografia líquida (HPLC) método para a determinação de cefixima tri-estresse sob diferentes condições, conforme especificado pelo ICH. Para a análise, a Phenomenex (250 x 4,6 mm, 5 µm de granulometria) ODS coluna e a SPD 20 um detector de UV em 289 nm foi utilizado. A fase móvel selecionado foi de 10 mM hidrogenofosfato dissódico (com 0,5% TEA, o pH ajustado para 6,3 com OPA) e de metanol em razão de 75:25 (v/v) no modo isocrático com uma taxa de fluxo de 1 mL.min-1. A análise de regressão linear para dados da calibração parcelas apresentaram boa relação linear com r2 = 0,9997 no intervalo de concentração de cerca de 5 100 µg.mL-1. Degradação do estresse foi realizado utilizando um ácido, alcalino, a água, o peróxido de hidrogênio e luz uv.

Quantitative estimation of (-)-hinokinin, a trypanosomicidal marker in Piper cubeba, and some of its commercial formulations using HPLC-PDA / 药物分析学报

The fruits of Piper cubeba have been used in Ayurvedic system of medicine for pain, tastelessness, painful urination and mouth diseases. Among its various chemical constituents, (-)-hinokinin, a trypanosomicidal dibenzylbutyrolactone lignan, is found in significant quantities. For quality evaluation of P. cubeba fruit and its commercial formulations, there is an urgent need to develop an analytical method based on (-)-hinokinin. For this purpose, an HPLC method was developed using photo diode array detector and Waters HR C18 column with gradient elution consisting of water and acetonitrile. The developed method was validated as per ICH-Q2B guidelines and found to be accurate, precise and linear over a wide range of concentrations (5–300 mg/mL). (-)-Hinokinin contents were found to be in the range of 0.005–0.109%(m/m) in various P. cubeba samples. The developed method was extended to LC–MS for further identification and characterization of (-)-hinokinin in samples. The developed method is simple, rapid and specific, and can be used as a tool for quality control of P. cubeba fruits and its commercial formulations.