scholarly journals Dual-mode gradient HPLC and TLC densitometry methods for the simultaneous determination of paracetamol and methionine in the presence of paracetamol impurities

Author(s):  
Hany Ibrahim ◽  
Abdallah M Hamdy ◽  
Hanan A Merey ◽  
Ahmed S Saad

Abstract Background Paracetamol is one of the most widely analgesic and antipyretic drugs recently integrated into the supportive therapy of COVID-19. The pharmaceuticals containing methionine with paracetamol may contribute to avoid hepatotoxicity and eventual paracetamol overdose-dependent death. Objective The current work purposes to develop and validate two chromatographic methods for the simultaneous determination of methionine and paracetamol in presence of two paracetamol impurities (4-nitrophenol and 4-aminophenol). Methods Two chromatographic methods were established and validated according to the International Conference on Harmonization guidelines. The first one was a RP-HPLC/UV method based on applying a “dual-mode” gradient elution. The separation was realized via varying both the composition of the ternary mobile phase (acetonitrile–methanol–water) and its flow rate. This strategy enabled a relatively rapid analysis with a satisfactory resolution, although the investigated compounds exhibit a significant difference in lipophilicity. The second one relied on TLC- densitometry, where the optimum separation was realized using a quaternary mobile phase system composed of butanol–dioxane–toluene–methanol (8: 2.5: 3.5: 0.3, by volume). Both methods were monitored at 220 nm. Results The developed methods were proven to be robust, accurate, specific, and appropriate for the routine analysis of paracetamol in its pure form or in pharmaceutical formulations with methionine in quality control laboratories. Conclusions The corresponding methods are suitable to determine methionine and paracetamol in the presence of paracetamol impurities. Highlights The study achieves the analysis of methionine and paracetamol in the presence of paracetamol impurities via the application of HPLC and TLC- densitometry methods.

Author(s):  
Nariman A. El-Ragehy ◽  
Maha A. Hegazy ◽  
Samia A. Tawfik ◽  
Ghada A. Sedik

Abstract Sulfacetamide sodium is a widely prescribed sulfonamide drug due to its topical antibacterial action on eye and skin. Four impurities are stated in the British Pharmacopoeia among which are sulfanilamide and dapsone. This work presents two specific, accurate and precise chromatographic methods for the simultaneous determination of a mixture of sulfacetamide sodium, sulfanilamide and dapsone. The first method is an isocratic RP-HPLC where the separation of components was achieved on C18 column. A green mobile phase was used consisting of methanol:water (60:40, v/v). The flow rate was 1.0 mL/min and effluent was monitored at 273 nm. The second method is a TLC-spectrodensitometric one where good separation was achieved by using silica plates and a mobile phase consisting of chloroform:dichloromethane:acetic acid (6:2.5:1.5, by volume). Determination was done by densitometry in the absorbance mode at 273 nm. Both methods were validated in compliance with ICH guidelines. They were also successfully applied for the determination of sulfacetamide sodium and its impurities in Ocusol® ophthalmic solutions. The obtained results were statistically compared to the results obtained by applying the official methods of analysis of each component where no significant difference was found with respect to accuracy and precision.


2015 ◽  
Vol 11 (8) ◽  
pp. 3850-3859 ◽  
Author(s):  
Basma Mohamed El-Tanany ◽  
Maha A. Hegazy ◽  
Medhat A. Al-Ghobashy ◽  
Fatma I. Khattab

Two chromatographic methods were developed and validated for the simultaneous determination of Sodium Cromoglycate (SCG) and Oxymetazoline Hydrochloride (OXMT). SCG and OXMT are administered in combination for effective treatment of nasal congestion and allergy. The first chromatographic method was based on usingaluminum TLC plates pre-coated with silica gel GF254 as the stationary phase and chloroform: methanol: toluene: triethylamine (5: 2: 4:1, by volume) as the mobile phase followed by densitometric measurement of the separated bands at 235 nm. The second method is a high performance liquid chromatographic method for separation and determination of SCG and OXMT using reversed phase C18 column with isocratic elution. The mobile phase composed of acetonitrile: methanol (2: 1, v/v) at flow rate of 1.0 mL/ min. Quantitation was achieved with UV detection at 220 nm. The validity of the proposed methods was assessed using the standard addition technique. The obtained results were statistically compared with those obtained by the official methods, showing no significant difference with respect to accuracy and precision at p = 0.05.


2019 ◽  
Vol 58 (1) ◽  
pp. 16-21
Author(s):  
Ibrahim A Naguib ◽  
Eman S Hassan ◽  
Aml A Emam ◽  
Eglal A Abdelaleem

Abstract Two selective and sensitive chromatographic methods were developed for simultaneous determination of new combination of quinfamide and mebendazole in bulk powder and in pharmaceutical formulation. The first method is HPTLC by which separation was obtained using silica gel HPTLC F254 plates and a simple mobile phase consisting of methanol:toluene (2:6, v/v) and the separated bands were scanned at 254 nm. The second method RP-HPLC that comprised isocratic separation of both drugs on a Phenomenex C18 column using a green mobile phase consisting of double distilled water:methanol (30:70, v/v) at a flow rate of 0.8 mL/min and UV detection at 254 nm. The developed methods were validated and proved to meet ICH guidelines. Successful application of the developed methods was carried out for determination of quinfamide and mebendazole in Vermox Plus® tablets. Statistical comparison between the developed chromatographic methods and the reported simultaneous equation spectrophotometric method showed that there was no significant difference between them, proving the ability of applying the proposed methods in quality control testing of the studied drugs. The developed methods are considered the first chromatographic methods for simultaneous determination of quinfamide and mebendazole; moreover, they offered sensitive and selective eco-friendly methods for analysis of the studied drugs.


2015 ◽  
Vol 98 (5) ◽  
pp. 1234-1239 ◽  
Author(s):  
Paula R Chellini ◽  
Eduardo B Lages ◽  
Pedro H C Franco ◽  
Fernando H A Nogueira ◽  
Isabela C César ◽  
...  

Abstract Tuberculosis treatment consists of a fixed dose combination of rifampicin (RIF), isoniazid (INH), pyrazinamide (PYZ), and ethambutol hydrochloride (EMB). The combined treatment using various drugs is necessary for patient curing, without recrudescence, and for prevention of drug-resistant mutants, which may occur during treatment. An HPLC-diode array detector (DAD) method for the simultaneous determination of RIF, INH, PYZ, and EMB in fixed dose combination tablets was developed and validated. Chromatographic experiments were performed on an Agilent 1200 HPLC system, and the separation was carried out on a Purospher STAR RP18e (250 × 4.6 mm id, 5 μm, Merck) analytical column. Gradient elution was carried out with a mobile phase of 20 mM monobasic sodium phosphate buffer with 0.2% triethylamine (pH 7.0) and acetonitrile at a flow rate of 1.5 mL/min. The total run time was 12 min, and the re-equilibration time was 5 min. EMB detection was performed at 210 nm, and RIF, INH, and PYZ were detected at 238 nm, using a DAD. The method proved to be specific, linear (r2 > 0.99), precise (RSD <2%), accurate, and robust and may be applied to the QC analysis of pharmaceutical formulations.


2013 ◽  
Vol 96 (6) ◽  
pp. 1273-1280 ◽  
Author(s):  
Suyog S Patil ◽  
Ashwini K Srivastava

Abstract A simple, precise, and rapid RPLC method has been developed without incorporation of any ion-pair reagent for the simultaneous determination of vitamin C (C) and seven B-complex vitamins, viz, thiamine hydrochloride (B1), pyridoxine hydrochloride (B6), nicotinamide (B3), cyanocobalamine (B12), folic acid, riboflavin (B2), and 4-aminobenzoic acid (Bx). Separations were achieved within 12.0 min at 30°C by gradient elution on an RP C18 column using a mobile phase consisting of a mixture of 15 mM ammonium formate buffer and 0.1% triethylamine adjusted to pH 4.0 with formic acid and acetonitrile. Simultaneous UV detection was performed at 275 and 360 nm. The method was validated for system suitability, LOD, LOQ, linearity, precision, accuracy, specificity, and robustness in accordance with International Conference on Harmonization guidelines. The developed method was implemented successfully for determination of the aforementioned vitamins in pharmaceutical formulations containing an individual vitamin, in their multivitamin combinations, and in human urine samples. The calibration curves for all analytes showed good linearity, with coefficients of correlation higher than 0.9998. Accuracy, intraday repeatability (n = 6), and interday repeatability (n = 7) were found to be satisfactory.


2011 ◽  
Vol 94 (5) ◽  
pp. 1427-1439
Author(s):  
Samah S Abbas ◽  
Nour E Wagieh ◽  
Mohamed Abdelkawy ◽  
Maha M Abdelrahman

Abstract Three methods are presented for the simultaneous determination of diloxanide furoate (DLX) and metronidazole (MTR), used for their antiprotozoal and antiamoebic effect, in the presence of DLX alkaline degradates and in pharmaceutical formulations, without previous separation. The first method is chemometric-assisted spectrophotometry, in which principal component regression and partial least squares were applied. These two approaches were successfully applied to quantify each drug in the mixture using the information included in the absorption spectra in the range of 225–320 nm. The second method is TLC-densitometry, in which the binary mixture and degradates were separated on silica gel plates using a chloroform–acetone–glacial acetic acid (9.5 + 0.5 + 0.07, v/v/v) mobile phase and the bands were scanned at 254 nm. The last method is HPLC, in which DLX, MTR, and degradates were separated using the mobile phase acetonitrile–0.05 M dibasic potassium phosphate (25 + 75, v/v), adjusted to pH 4 with orthophosphoric acid, at a flow rate of 1 mL/min, on a C18 analytical column. Detection was at 254 nm. The proposed methods were successfully applied for the analysis of DLX and MTR in pharmaceutical formulations, and the results were statistically compared with a reported spectrophotometric method.


2012 ◽  
Vol 581-582 ◽  
pp. 68-72
Author(s):  
Chu Qin Yu ◽  
Hua Qing Lin ◽  
Yue Han Hou ◽  
Zhong Feng Shi ◽  
Di Shi Lin

In this study, our purpose was to establish a UPLC method for the simultaneous determination of Paeoniflorin and Paeonol in Houyinan Tablet. The separation was performed on Acquity BEH C18 column(2.1mm×100mm,1.7μm), the mobile phase was acetonitrile-water with gradient elution at a flow rate of 0.2 mL•min-1, the detection wavelength was 230nm, the column temperature was 30°Cand the injection volume was 2μL. Paeoniflorin and Paeonol reached effective separation with the other components in this chromatographic conditions. Paeoniflorin and Paeonol were linear within the range of 0.0406~0.4064μg(r=0.9999) and 0.0426~0.4256μg (r=0.9999), respectively. The average recovery was 99.82% and 100.6%. The results of method validation indicated that the method was simple,quick,accurate, specific and less solvent consumption. It can be used for the quality control of Houyinan Tablet.


2020 ◽  
Vol 66 (1) ◽  
pp. 85-90
Author(s):  
Zhaklina Poposka Svirkova ◽  
Zorica Arsova-Sarafinovska ◽  
Aleksandra Grozdanova

Due to the low absorptivity of bile acids, the aim of this study was to develop and validate a simple and sensitive HPLC/UV method for quantification of ursodeoxycholic acid (UDCA) in pharmaceutical formulations. Effective separation was achieved on C18 end–capped column, with gradient elution of a mobile phase composed of 0.001 M phosphate buffer (pH 2.8±0.5) – acetonitrile mix, at flow rate 1.5 mL min-1, UV detection at 200 nm and injection volumes were 50 µL. The proposed HPLC method was fully validated according to the ICH guidelines and it was found to be simple, accurate, precise and robust. Key words: ursodeoxycholic acid, HPLC/UV, pharmaceutical formulations, validation


2013 ◽  
Vol 96 (2) ◽  
pp. 313-323 ◽  
Author(s):  
Rasha M Youssef ◽  
Hadir M Maher ◽  
Eman I El-Kimary ◽  
Ekram M Hassan ◽  
Magda H Barary

Abstract Two stability-indicating chromatographic methods are described for simultaneous determination of amiloride hydrochloride (AMI), atenolol (ATE), and chlorthalidone (CHL) in combined dosage forms. The first method was based on HPTLC separation of the three drugs followed by densitometric measurements of their bands at 274 nm. The separation was carried out on Merck HPTLC silica gel 60F254 aluminum sheets using chloroform–methanol–ammonia 27%, w/w (9 + 2 + 0.3, v/v/v) mobile phase. Analysis data was used for the linear regression graph in the range of 0.1–0.5, 0.8–5.0, and 0.3–1.5 μg/band for AMI, ATE, and CHL, respectively. The second method was based on an RP-HPLC separation of the cited drugs performed on an RP stainless steel C18 analytical column (250 × 4.6 mm id) with a gradient elution system of methanol and 0.05 M aqueous phosphate buffer adjusted to pH 4 as the mobile phase, at the flow rate of 1.0 mL/min. Quantitation was achieved with photodiode array detection at 275 nm for AMI and 225 nm for ATE and CHL. The calibration graphs for each drug were rectilinear in the range of 2–50, 25–150, and 2–100 μg/mL for AMI, ATE, and CHL, respectively. The proposed chromatographic methods were successfully applied for determination of the investigated drugs in pharmaceutical preparations. Both methods were validated in compliance with International Conference on Harmonization guidelines in terms of linearity, accuracy, precision, robustness, LOD, and LOQ.


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