scholarly journals SIMULTANEOUS QUANTIFICATION OF PENTAZOCINE AND NALOXONE BY STABILITY INDICATING REVERSE-PHASE-HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD

Author(s):  
RAMA KUMAR KANDULA ◽  
RAJA SUNDARARAJAN

Objective: The objective of the study was to develope a stability indicating high-performance liquid chromatographic (HPLC) method for simultaneous assay of pentazocine and naloxone in bulk and tablets. Methods: Pentazocine and naloxone were analyzed on Dionex C18 column using 0.1M K2HPO4 buffer (pH 4.0) and methanol (60:40, v/v) as the mobile phase. The concentration of pentazocine and naloxone was quantified by photodiode array detector set at 248 nm. The method was validated in compliance with ICH rules. Pentazocine and naloxone tablet formulation was subjected to forced degradation such as acid, neutral and alkali hydrolysis, oxidation, photo, and thermal degradation. Results: The method was linear, with R2=0.9999 in the concentration range 100–300 μg/ml for pentazocine and R2=0.9995 in the concentration range 1–3 μg/ml for naloxone. The level of detection and quantification was 0.097 μg/ml and 0.322 μg/ml for pentazocine and 0.0073 μg/ml and 0.0243 μg/ml for naloxone, respectively. The degraded products are resolved well from pentazocine and naloxone with significantly different retention time values. From validation results, it was proved that the method is selective, precise, robust, and accurate for the estimation of pentazocine and naloxone simultaneously. Conclusion: The developed stability-indicating HPLC method can be applied for quantitative determination of pentazocine and naloxone in tablets.

Author(s):  
Saniye Özcan ◽  
Serkan Levent ◽  
Nafiz Öncü Can

: The alkyl esters of p-hydroxybenzoic acid at the C-4 position, “the parabens,” including methyl, ethyl, propyl, and butyl, are widely used as antimicrobial preservatives in foods, cosmetics, and pharmaceuticals. Official regulations on the use of these compounds make their analysis essential for the estimation of their exposure. On this basis, the presented study was realized to develop a simple, selective and cheap high-performance liquid chromatographic method for the quantitative determination of methyl paraben (MP), ethyl paraben (EP), n-propyl paraben (NPP), isopropyl paraben (IPP), n-butyl paraben (NBP), isobutyl paraben (IBP) and benzyl paraben (BP) in pharmaceuticals and cosmetic products. The chromatographic separation of the analytes was achieved under flow rate gradient elution conditions using a C18-bonded core-shell silica particle column (2.6 μm particle size, 150 × 3.0 mm from Phenomenex Co.). The samples were injected into the system as aliquots of 1.0 μL, and the compounds were detected by using a photodiode array detector set at 254 nm wavelength. With this technique, seven paraben derivatives can be determined in the concentration range of 250-2000 ng/mL. The recovery of the method is in the range of 99.95-13.84%, and the RSD is at a maximum value of 3.95%. The proposed method was fully validated and successfully applied to different pharmaceutical and cosmetic samples (n=16), including syrups, suspensions, oral sprays, gels, etc. At least one paraben derivative was detected in six of the samples, and was determined quantitatively. The maximum amount of a paraben derivative found in the analyzed samples is 321.7 ng/mL, which was MP. To the best of our knowledge, this is the first LC method, which is applicable both on pharmaceutical and cosmetic samples.


2010 ◽  
Vol 7 (s1) ◽  
pp. S299-S313 ◽  
Author(s):  
P. Shetti ◽  
A. Venkatachalam

A new, simple, precise, rapid, selective and stability indicating reversed-phase high performance liquid chromatographic (HPLC) method has been developed and validated for simultaneous quantification of trihexyphenidyl hydrochloride, trifluoperazine hydrochloride and chlorpromazine hydrochloride from combined tablet formulation. The method is based on reverse-phase using C-18 (250×4.6) mm, 5 μm particle size column. The separation is achieved using isocratic elution by methanol and ammonium acetate buffer (1% w/v, pH 6.5) in the ratio of 85:15 v/v, pumped at flow rate 1.0 mL/min and UV detection at 215 nm. The column is maintained at 30 °C through out the analysis. This method gives baseline resolution. The total run time is 15 min. Stability indicating capability is established buy forced degradation experiment. The method is validated for specificity, accuracy, precision and linearity as per International conference of harmonisation (ICH). The method is accurate and linear for quantification of trihexyphenidyl hydrochloride, trifluoperazine hydrochloride and Chlorpromazine hydrochloride between 5 - 15 μg/mL, 12.5- 37.5 μg/mL and 62.5 - 187.5 μg/mL respectively.


2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Anuradha Vejendla ◽  
Subrahmanyam Talari ◽  
Raju Moturu ◽  
S. N. Murthy Boddapati ◽  
A. Emmanuel Kola

Abstract Background Using a Symmetry C18 (4.6 × 150 mm, 3.5) column, a high-performance liquid chromatographic method for quantification of Rilpivirine and Cabotegravir in active pharmaceutical ingredients was developed and validated. The mobile phase is made up of buffer, acetonitrile, and 0.1 percent formic acid in a 20:80v/v ratio. The flow rate was kept constant at 1.0 ml/min, and detection was accomplished through absorption at 231 nm with a photodiode array detector. Results The calibration curve was linear, with a regression coefficient (R2) value of 0.999 and concentrations ranging from 30 to 450 g/ml of Rilpivirine and 20–300 g/ml of Cabotegravir. The method's LOD and LOQ were 0.375 g/ml, 1.238 g/ml, and 0.25 g/ml, 0.825 g/ml for Rilpivirine and Cabotegravir, respectively. Conclusions In the forced degradation studies, the degradants were characterized by using LCMS and FTIR. The current application was found to be simple, economical, and suitable, and validated according to ICH guidelines.


2016 ◽  
Vol 8 (30) ◽  
pp. 5949-5956 ◽  
Author(s):  
Soumia Boulahlib ◽  
Ali Boudina ◽  
Kahina Si-Ahmed ◽  
Yassine Bessekhouad ◽  
Mohamed Trari

In this study, a rapid and simple method based on reversed-phase high performance liquid chromatography (RP-HPLC) using a photodiode array detector (PDA) for the simultaneous analysis of five pollutants including aniline and its degradation products, para-aminophenol, meta-aminophenol, ortho-aminophenol and phenol, was developed.


INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (04) ◽  
pp. 48-55
Author(s):  
S. Jadhav ◽  
◽  
P. Pisal ◽  
M. Mahajan

A stability indicating RP-HPLC method has been developed and subsequently validated for Sirolimus. The proposed RP-HPLC method utilizes Phenomenex, C18, 3 μm, 4 mm x 150 mm column, mobile phase consisting of acetonitrile and water (65:35 V/V) and UV detection at 277 nm using a photodiode array detector in the stressed sample chromatograms. Crushed sirolimus tablets were exposed to thermal, photolytic, aqueous and oxidation stress conditions and stressed samples were analysed by the proposed method. Peak homogeneity data of the drug peaks were obtained using photodiode array detector. The stressed sample chromatograms demonstrated the specificity of the method for their estimation in presence of degradants. 99.66% degradation was observed in acid degradation study. on the other hand, no degradation was observed in aqueous condition. The given method was linear over a range of 0.1566 mg/mL to 0.4699 mg/mL. The mean recovery was found to be 99.23%. Acid degradant was separated by HPTLC and spectroscopic analysis was performed for the same.


2016 ◽  
Vol 9 (1) ◽  
pp. 54
Author(s):  
Megha Sharma ◽  
Neeraj Mahindroo

Objective: The objective of the present study was to develop and validate a novel stability indicating reverse phase-high performance liquid chromatography (RP-HPLC) method for determination of β-acetyldigoxin, an active pharmaceutical ingredient (API).Methods: The chromatographic separation was carried out on Agilent Technologies 1200 series HPLC system equipped with photo diode array detector and C-18 (4.6x250 mm, 5 µ) column. The mobile phase consisted of water: acetonitrile (65:35 v/v), delivered at a flow rate of 1.5 ml/min and eluents were monitored at 225 nm.Results: The retention time of β-acetyldigoxin was 9.2 min. The method was found to be linear (R2= 0.9995) in the range of 31.25-500 µg/ml. The accuracy studies showed the mean percent recovery of 101.02%. LOD and LOQ were observed to be 0.289 µg/ml and 0.965 µg/ml, respectively. The method was found to be robust and system suitability testing was also performed. Forced degradation analysis was carried out under acidic, alkaline, oxidative and photolytic stress conditions. Significant degradation was observed under tested conditions, except for oxidative condition. The method was able to separate all the degradation products within runtime of 20 min and was able to determine β-acetyldigoxin unequivocally in presence of degradation products.Conclusion: The novel, economic, rapid and simple method for analysis of β-acetyldigoxin is reported. The developed method is suitable for routine quality control and its determination as API, and in pharmaceutical formulations and stability study samples.


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