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temperature was maintained at constant 35°C using a CTO-20A column oven. Method validation Standard solutions were prepared by dissolving reference substances (HM and PM) at six different concentrations and analyzed by HPLC with injection volumes of 10 μL. The

Open access
Acta Chromatographica
Authors: Fatema Moni, Suriya Sharmin, Satyajit Roy Rony, Farhana Afroz, Shammi Akhter, and Md. Hossain Sohrab

collected, transferred to autosampler vials and directly injected into HPLC. Method validation The rationale of analytical method development is to provide consistent, reliable, and accurate data. For this reason, the performances and the limitations of the

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Summary

Herein, the isolation, characterization, and method validation of 5 bioactive terpenoids, viz., taraxerol (1), 3ß-hydroxyoleanane-12-one (2), betulinic acid (3), ursolic acid (4), and oleanolic acid (5) from Codonopsis ovata has been reported. A novel, accurate, and cost-effective high-performance thin-layer chromatography method was developed for the simultaneous quantification of 5 natural products on silica-gel 60 F254 plate using a ternary solvent system, n-hexane-ethyl acetate-formic acid (8.0:2.0:0.4, V/V). Markers were quantified after post-chromatographic derivatization with ceric ammonium sulfate reagent. The developed method was validated as per the International Conference on Harmonization (ICH) guidelines. All calibration curves showed a good linear relationship (r > 0.995) within the test range. Precision was evaluated by intra- and inter-day tests with relative standard deviations <1.99%, and accuracy validation recovery 85.66–91.87 with relative standard deviations >2.00°%. Oleanolic acid (5) and ursolic acid (4) were found in major quantity which is advantageous because of their anticancer, anti-inflammatory, anti-mutagenic, and anti-obesity activities. Based on our results, the developed method features good quantification parameters and can serve as an effective quality control method for standardization of Codonopsis ovata.

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Summary

Linear gradient HPLC on a C8 column has been used for separation of individual related substances of amoxicillin listed in the European Pharmacopoeia and a newly identified degradation impurity. The USP plate count for the amoxicillin peak was more than 3000 and USP tailing for the same peak was less than 2.0. Forced degradation studies were conducted on amoxicillin drug substance using ICH stress study guidelines to demonstrate the specificity and stability-indicating nature of the method. A new impurity observed after thermal and alkaline degradation was identified as N-pivaloylamoxicillin. The LOD and LOQ for individual related substances were below 0.045 and 0.086% (w/w), respectively. The method was fully validated in accordance with ICH analytical method validation guidelines. The results of the study prove the method is specific, precise, linear, robust, and can be used for evaluation of the stability of amoxicillin drug substance.

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Hz; cone voltage, 15 V; source temperature, 120 °C; and turbo temperature, 45 °C. The selective ion recording (SIR) of DPT was monitored at m / z 421 in positive mode. Method Validation The DPT standard compound

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Statistics: Fundamentals of Clinical Pharmacokinetics Drug Intelligence Publications Hamilton 285 . [18]. USFDA , Guidance for Industry: Bioanalytical Method

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/mL by considering their toxicity value. Method Validation The developed analytical method was validated for its acceptable performance to ensure suitability of indent purpose. The validation parameters like accuracy

Open access

Summary

A simple, rapid, precise, and accurate, stability-indicating reversed phase high performance liquid chromatographic method was developed and validated for simultaneous determination of metformin HCl and repaglinide. The chromatographic separation was achieved on YMC Pack AM ODS (5 μm, 250 mm length × 4.6 mm i.d.) column at a detector wavelength of 210 nm, using an isocratic mobile phase consisting of methanol and 10 mM potassium dihydrogen phosphate buffer (pH 2.5) in a ratio of 70:30 v/v at a flow rate of 1 mL min−1. The retention times for metformin and repaglinide were found to be 2.6 and 11.3 min, respectively. The drugs were exposed to thermal, photolytic, hydrolytic, and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. Validation of the method was carried out as per International Conference on Harmonization (ICH) guidelines. Linearity was established for metformin and repaglinide in the range of 5–200 μg mL−1 and 1–200 μg mL−1, respectively. The limits of detection were 0.3 μg mL−1 and 0.13 μg mL−1 for metformin and repaglinide, respectively. The method was found to be specific and stability-indicating as no interfering peaks of degradants and excipients were observed. The proposed method is hence suitable for application in quality-control laboratories for quantitative analysis of both the drugs individually and in combination, since it is simple and rapid with good accuracy and precision.

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Acta Chromatographica
Authors: Lenche Velkoska-Markovska, Mirjana S. Jankulovska, Biljana Petanovska-Ilievska, and Kristijan Hristovski

. Method Validation Validation of the method for determination of chlorogenic acid in green coffee was performed testing following parameters: linearity, specificity, selectivity, precision, accuracy, limit of detection (LOD), and limit of

Open access

Abstract  

For the determination of 210Po in water samples, two alternative procedures (a) DDTC solvent extraction and (b) extraction chromatography using Sr Resin were selected and then validated in terms of trueness, repeatability and reproducibility with a tap water spiked with a known amount of 210Po. In this work the optimization conditions for the auto-deposition of Po for source preparation were also studied.

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