Stability-indicating HPTLC determination of capsaicin in the bulk drug (original) (raw)
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Pharmaceutical Methods, 2011
Background: Stability Indicating Method (SIM) is a quantitative analytical procedure used to detect a decrease in the amount of the active pharmaceutical ingredient (API) present due to degradation. According to Food and Drug Administration (FDA) guidelines, an SIM is defined as a validated analytical procedure that accurately and precisely measures active ingredients (drug substance or drug product) free from potential interferences, such as degradation products, process impurities, excipients, or other potential impurities, and the FDA recommends that all assay procedures for stability studies be stability indicating. Here in this study we developed simple precise and accurate stability indicating reverse-phase high-performance liquid chromatographic (RP-HPLC) assay to analyze capsaicin (CAP) at concentrations from 70 to 130 µg/mL. Materials and Methods: HPLC equipped with Photo diode Array (PDA) detector, Pump model 600E of Waters and Empower software. Column used for the separation is ODS (250 × 4.6 mm) with particle size 5 µm and all the reagents and water were of HPLC grade. Results: The chromatographic separation was carried out using mobile phase Acetonitrile (ACN):water:buffer::75:10:15 with a flow rate of 1 mL/min on a C18 column. The concentration of the eluting compounds was monitored by a UV detector at 280 nm. No interferences were observed when stress conditions were applied and analyzed. Linearity was established using visual method, residuals plot, Dixon, and lack of fitness test. Limit of detection and limit of quantification was found to be 52.9 and 160 ng/mL, respectively. Recovery studies prove this method as useful in recovering the analytes. Relative Standard Deviation (RSD) of inter-and intraday precision within the acceptable limit of 2% proves that this method is precise. No degradation was found with alkaline conditions, thermal and photodegradation. Conclusions: This study can be used for successful separation of CAP and its potential degradants in bulk and formulations. UV spectra of one of the degradants are also presented here and can be the basis to generate chemistry of potential degradants when CAP is kept under environmental conditions.
Recent applications of LC-MS in the analysis of drug degradation products in pharmaceutical formulations are reviewed. Drug degradation products are categorized according to their formation mechanism: oxidation, hydrolysis, dimerization and adduct formation with excipients and packaging materials. The oxidative ring opening and dimerization of an indole derivative are discussed in detail. The examples used in this review clearly demonstrate that LC-MS is a very powerful technique for the analysis of low-level degradates in formulations without the time-consuming isolation process. At the same time, limitations and precaution of using LC-MS techniques for unknown identification are also addressed. In some cases, the LC-MS data could become misleading if the ionization process and gas-phase behavior of the analytes are not well understood. Identification of drug degradation products REVIEW ARTICLE Figure 2. Product ion spectra of the major degradates of compound II. (A). Compound IV in the negative ion mode; (B) compound IV in the positive ion mode; (C) compound V in the positive ion mode; (D) compound III in the positive ion mode. (figs 2-4 were acquired on a PE-Sciex API-300 mass spectrometer with a TurboIonSpray interface.) Scheme 4. Fragmentation mechanism for the diacid (IV) in the negative ion mode.
Stability Indicating HPLC Determination of Clopidogrel bisulphate in Pharmaceutical Dosage forms
However, most of these methods either require very expensive instruments and reagents or complicated procedures. Hence, there is a need for simple, rapid and reproducible method for the routine analysis of pharmaceutical dosage forms. The aim of the present work is to develop simple, accurate, reproducible and stability indicating method for the determination of Clopidogrel in the presence of its degradation products and related impurities as per ICH guidelines. MATERIALS AND METHODS Chemicals and Reagents Clopidogrel bisulfate was supplied by Sun Pharmaceutical Industries Limited, Gujarat. Acetonitrile HPLC grade was procured from Avantor Performance Materials, Philipsberg, USA. High purity water was prepared with Elix-milli-Q system. Acetic acid GR procured from Merck, Germany. Sodium hydroxide, hydrochloric acid and hydrogen peroxide were procured from Qualigens, India. Instrumentation The HPLC instrument used was AGILENT 1260 RRLC system equipped with a photodiode array detector PDA 1290 infinity. Chromatographic Conditions Chromatographic separation was achieved on a reverse phase column Phenomenax C 18 (250 × 4.6 mm, 5µ) at ambient temperature using a mobile phase consisting of a mixture of Acetonitrile and Acetic acid (0.1% aqueous solution) in the ratio of (85:15) at a flow rate of 1ml/min.
Chromatographia, 2009
A novel stability-indicating LC assay method was developed and validated for quantitative determination of olmesartan in bulk drugs and in pharmaceutical dosage form in the presence of degradation products generated from forced degradation studies. An isocratic, reversed phase LC method was developed to separate the drug from the degradation products, using an Ace5-C18 (250 mm 9 4.6 mm, 5 lm) column, and 50 mM ammonium acetate (pH-5.5 by acetic acid) and acetonitrile (70:30 v/v) as a mobile phase. The detection was carried out at the wavelength of 235 nm. The olmesartan was subjected to stress conditions of hydrolysis (acid, base), oxidation, photolysis and thermal degradation. Degradation was observed for olmesartan in acid, base and in 30% H 2 O 2 conditions. The drug was found to be stable in the other stress conditions attempted. The degradation products were well resolved from the main peak. The percentage recovery of olmesartan ranged from (99.89 to 100.95%) in pharmaceutical dosage form. The developed method was validated with respect to linearity, accuracy (recovery), precision, specificity and robustness. The forced degradation studies prove the stability-indicating power of the method.
Recent applications of analytical techniques for quantitative pharmaceutical analysis: A review
2010
The intension of this paper was to review and discuss some of the current quantitative analytical procedures which are used for quality control of pharmaceutical products. The selected papers were organized according to the analytical technique employed. Several techniques like ultraviolet/visible spectrophotometry, fluorimetry, titrimetry, electroanalytical techniques, chromatographic methods (thin-layer chromatography, gas chromatography and high-performance liquid chromatography), capillary electrophoresis and vibrational spectroscopies are the main techniques that have been used for the quantitative analysis of pharmaceutical compounds. In conclusion, although simple techniques such as UV/VIS spectrophotometry and TLC are still extensively employed, HPLC is the most popular instrumental technique used for the analysis of pharmaceuticals. Besides, a review of recent works in the area of pharmaceutical analysis showed a trend in the application of techniques increasingly rapid such as ultra performance liquid chromatography and the use of sensitive and specific detectors as mass spectrometers.
Development and validation of HPLC-UV method for the estimation of fulvestrant in bulk drug
Aim: The present work is aimed to develop a simple, rapid, selective, sensitive and validated HPLC method for the determination of fulvestrant in bulk drug. Method: Fulvestrant was measured using a validated HPLC method with UV detector at 225nm chromatographic peaks were separated on Phenomix, C18 column (250 mm x 4.6 mm x3.5µ) using 50% aetonitrile in channel A and acetonitlile in channel B as mobile phase with gradient elution at a flow rate of 1 ml/min. Results & Discussions: The chromatograms showed good peak shapes and no interference of solvent peaks. The retention time of fulvestrant was found to be 13.6 min. LOD and LOQ were found to be 0.0226µg/ml (0.001%) and 0.0712µg/ml,(0.004%) respectively. The percentage recovery of fulvestrant was found to be 99.1% - 100.75% which are within the limit. The method was linear over the concentration range of 0.08to 2ìg/ml with coefficient of correlation (r2) 0.99997. Both intraday and inter day accuracy and precision data showed good reproducibility. Conclusions: The low % RSD values (= 2) indicated that the method was precise and accurate. this method was successfully applied to forced degradation studies and can be adopted for routine estimation of fulvestrant in quality control laboratories.
Journal of Liquid Chromatography & Related Technologies, 2009
This work studies the stability of three new anti-HIV agents which were obtained by the association of zidovudine (AZT) with different amino acids, such as leucine (AZT-Leu) and valine (AZT-Val), and one with an acid group (AZT-Ac). Before commercialisation, their stability in different matrices -simulated gastric fluid (SGF, pH 1.2) and simulated intestinal fluid (SIF, pH 6.8), both as the USP 32 Guideline indicates, and buffers (pH 1.2 and 6.8) -must be studied. To this end, a new stability-indicating micellar liquid chromatography (MLC) method has been optimised and validated. Measurements were based on the disappearance of reagents and the appearance of the only degradation product (AZT). This optimised and validated method used a C18 column and a mobile phase containing 0.05 M sodium dodecyl sulphate-1% (v/v)1-butanol-0.01 M NaH 2 PO 4 (pH 3.0) at 30 • C, and a flow rate of 1 mL min −1 . Under these conditions, retention times were 1.4, 3.6, 6.3 and 9.5 min for AZT-Ac, AZT, AZT-Val and AZT-Leu, respectively. Calibrations better than 0.9995, intra-and inter-day precisions below 1.08% and good recoveries (94.47-116.52%) and robustness (RSD less that 1.08%) were obtained and were adequate to analyse the four compounds. Finally, this MLC method was applied to achieve stability studies which resulted in the evidence that all the compounds followed a pseudo-first-order kinetics, and in the determination of their kinetic constants and half-life time. A reference method, applied in the same studies, validated the MLC method reported herein.
Practical advance pharmaceutical analysis
1. Fundamentals of Spectrophotometer (Assay of tetracycline by calibration curve method). 2. Spectrophotometric determination of (Aspirin in tablets By standard addition method). 3. Fundamentals of Infrared Spectroscopy (Sold and liquid). 4. Application of IR Spectroscopy in the Analysis of Pharmaceutical Substances 5. Titration of the Ascorbic acid (vitamin C) in tablets By pH meter used first and 2nd derivatives. 6. Multi-Component Analysis of a Vitamin B Mixture by UV-Vis. Spectroscopy 7. Determination of Caffeine and Acetylsalicylic Acid in an Analgesic Tablet 8.UV-Vis. Spectroscopy Calibration 9. Spectrophotometric (Determination of Iron in a Vitamin Tablet) 10. Flame Photometer (Determination of Na & K in Tablet)
RP-HPLC Method Development and Validation for the Analysis of Pharmaceutical Drugs
International Journal of Science and Research (IJSR), 2016
A simple, selective, linear, precise and accurate RP-HPLC method was developed and validated for rapid assay of PARACETAMOL. Isocratic elution at a flow rate of 1.0 ml /min was employed on a symmetry C18 column at ambient temperature. The mobile phase consisted of Acetonitrile: 0.1M Acetic Acid 50:50 (v/v). The UV detection wavelength was at 210 nm. Linearity was observed in concentration range of 100-140 mg/ml. The retention time for Paracetamol was 3.0 min. The method was validated as per the ICH guidelines. The proposed method can be successfully applied for the estimation of Paracetamol.
A HPTLC/Densitometric method has been developed for the determination of Guaifenesin (GFN) in bulk and pharmaceutical formulation. The estimation of drug was performed on HPTLC aluminium plates precoated with silica gel 60 RP-18 TLC F254 S using toluene: methanol: ethyl acetate: acetic acid (7:0.8:1.2:0.5 v/v/v/v) as mobile phase. The densitometric quantification for the drug was carried out at 274 nm. GFN obeyed linearity in concentration range 800 – 2800 ng/band with coefficient of correlation 0.999. The Rf for GFN was found to be 0.6 ± 0.02. The proposed method was applied for pharmaceutical formulation and % label claim for GFN was found to be 100.34 1.06. The method was validated for accuracy, precision and ruggedness. Accuracy of the method was checked by recovery studies at three different levels i.e. 80 %, 100 % and 120 %. The % recovery of GFN was found to be in the range of 99.48% - 100.68 %; the % RSD value was less than 2 indicates the accuracy of the method. The method was found to be precise as indicated by the inter-day, intra-day and repeatability analysis; showing % RSD less than 2. The results did not show any statistical difference between operators showing that developed method was rugged. GFN was subjected to acid and alkali hydrolysis, oxidation and thermal degradation. The drug undergoes degradation under acid-base conditions, hydrolysis, oxidation, photo degradation except dry heat degradation. This indicates that the drug is susceptible to acid and base. The degraded product was well resolved from the pure drug with significantly different Rf value. Statistical analysis proves that the method is repeatable, selective and accurate for the estimation of investigated drug. The proposed developed HPTLC method can be applied for the identification and quantitative determination of GFN in bulk drug and pharmaceutical formulation.