Implementation of Two Chromatographic Methods for Simultaneous Quantitation of Thioctic Acid, Benfotiamine and Cyanocobalamin

2021 ◽  
Author(s):  
Samah S Abbas ◽  
Amr M Badawey ◽  
Maryam A Bakr ◽  
Maha A Hegazy
Keyword(s):  
Mobile Phase ◽  
Reversed Phase ◽  
Retardation Factor ◽  
Thioctic Acid ◽  
Rapid Separation ◽  
Chromatographic Methods ◽  
Ich Guidelines ◽  
Significant Difference ◽  
Rf Values ◽  
Liquid Chromatographic

Abstract Two accurate and sensitive chromatographic methods have been introduced and validated for the simultaneous determination of thioctic acid, benfotiamine and cyanocobalamin in bulk powders and in their pharmaceutical formulation. Method A is reversed-phase ultra performance liquid chromatographic method with an isocratic elution, where a rapid separation was accomplished on a Zorbax C8 column using a mobile phase of acetonitrile:0.05 M phosphate buffer (pH 6 adjusted by o-phosphoric acid) (23:77, v/v). The retention times (tR) were 0.578, 0.852 and 1.376 for cyanocobalamin, benfotiamine and thioctic acid, respectively. The separated peaks were revealed at 210.0 nm. Method B is a thin-layer densitometric method where the separation of the studied drugs was carried out on silica gel plates using methanol–chloroform–heptane-1-sulphonic acid sodium salt (0.4%) (7:3:0.1, by volume) as a mobile phase, and scanning of the separated bands was done at 240.0 nm. The retardation factor (Rf) values were 0.17, 0.48 and 0.75 for cyanocobalamin, benfotiamine and thioctic acid, respectively. Validation of the methods was achieved following ICH guidelines and the applied methods succeeded to determine the cited drugs in their pure forms and capsules. Results were statistically compared to the manufacturer’s method where no significant difference was observed.

Green Liquid Chromatographic Methods with Ultraviolet and Tandem Mass Spectrometry Detection: An Application to Ternary Mixture of Paracetamol, Pseudoephedrine, and Cetirizine in Capsules

2020 ◽  
Vol 103 (1) ◽  
pp. 148-155 ◽  
Author(s):  
Souha H Youssef ◽  
Dalia Mohamed ◽  
Maha A Hegazy ◽  
Amr Badawey
Keyword(s):  
Mobile Phase ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Hplc Method ◽  
Green Solvents ◽  
Chromatographic Methods ◽  
Combination Methods ◽  
Significant Difference ◽  
Acid Aqueous Solution ◽  
Liquid Chromatographic

Abstract Background: Effective chromatographic methods were developed for the determination of a multicomponent capsule prescribed for treating the common cold. Greening approaches were adopted as opposed to conventional methods. Objectives: Two novel, green chromatographic methods were established to quantitatively analyze the combination. Methods: First, an HPLC/UV method utilizing green solvents (water and ethanol) and acetic acid to adjust pH at 5 was accomplished. The stationary phase was a ZorbaxSB-C18 column (150 × 4.6 mm, 5 μm), and peaks were detected at 215 nm. The second method is a highly sensitive ultra-performance LC (UPLC)-MS/MS method in which the greening approach was established through the reduction of the analysis time (2 min), decreased solvent consumption (flow rate 300 μL/min), and the utilization of a small volume of samples (injection volume 2 μL). The mixture was separated using a UPLC-BEH C18 column (50 × 2.1 mm, 1.7 μm) with an isocratic elution using methanol–0.1% formic acid aqueous solution (60+40, v/v) as mobile phase and utilizing diphenhydramine as an internal standard. Positive-ion electrospray ionization and multiple reaction monitoring were applied for detection. Results: Recovery percentages for paracetamol, pseudoephedrine, and cetirizine were 101.70 ± 0.969, 100.18 ± 1.563, and 99.67 ± 1.429 for the HPLC method and 99.18 ± 1.172, 100.03 ± 0.883, and 99.82 ± 0.912 for the UPLC-MS/MS method, respectively. Conclusions: The proposed methods efficiently analyzed paracetamol, pseudoephedrine, and cetirizine in Allercet Cold® capsules. Validation of the proposed methods was in accordance with the International Conference on Harmonization recommendations, and statistical comparison with the reported method displayed no significant difference regarding accuracy and precision. Highlights: Paracetamol, pseudoephedrine, and cetirizine were successfully quantified using two chromatographic methods. The HPLC method developed is considered green, using water and ethanol as a mobile phase. The UPLC-MS/MS method was rapid and determined the three drugs with accuracy at nanogram levels.

scholarly journals Validated chromatographic methods for the simultaneous determination of a ternary mixture of sulfacetamide sodium and two of its official impurities; sulfanilamide and dapsone

2021 ◽  
Author(s):  
Nariman A. El-Ragehy ◽  
Maha A. Hegazy ◽  
Samia A. Tawfik ◽  
Ghada A. Sedik
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Volume Determination ◽  
Chromatographic Methods ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Significant Difference ◽  
Topical Antibacterial ◽  
Sulfacetamide Sodium

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.

scholarly journals Validated Chromatographic Methods for the Simultaneous Determination of Sodium Cromoglycate and Oxymetazoline Hydrochloride in a Combined Dosage Form

2015 ◽  
Vol 11 (8) ◽  
pp. 3850-3859 ◽  
Author(s):  
Basma Mohamed El-Tanany ◽  
Maha A. Hegazy ◽  
Medhat A. Al-Ghobashy ◽  
Fatma I. Khattab
Keyword(s):  
Sodium Cromoglycate ◽  
Simultaneous Determination ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Nasal Congestion ◽  
Standard Addition ◽  
Reversed Phase ◽  
Chromatographic Methods ◽  
Significant Difference

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.

Development and Validation of HPTLC and Green HPLC Methods for Determination of a New Combination of Quinfamide and Mebendazole

2019 ◽  
Vol 58 (1) ◽  
pp. 16-21
Author(s):  
Ibrahim A Naguib ◽  
Eman S Hassan ◽  
Aml A Emam ◽  
Eglal A Abdelaleem
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Simultaneous Equation ◽  
New Combination ◽  
Chromatographic Methods ◽  
Ich Guidelines ◽  
Quality Control Testing ◽  
Significant Difference ◽  
Development And Validation

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.

Resolution and Quantitation of Triamcinolone Acetonide and Its Coformulated Drug in the Presence of Its Impurities and Degradation Products by HPTLC and HPLC

2018 ◽  
Vol 101 (4) ◽  
pp. 981-991
Author(s):  
Samah S Abbas ◽  
Maha A Hegazy ◽  
Hassan A M Hendawy ◽  
Soheir A Weshahy ◽  
May H Abdelwahab
Keyword(s):  
Triamcinolone Acetonide ◽  
Mobile Phase ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Ich Guidelines ◽  
System Suitability ◽  
Significant Difference

Abstract Two specific, sensitive, and precise stability-indicating chromatographic methods have been developed for the determination of triamcinolone acetonide (TMC) and its coformulated drug, econazole nitrate (ECZ), in the presence of TMC impurities and degradation products. The first method was based on HPTLC-spectrodensitometry in which resolution and quantitation was achieved by using silica gel 60 F254 HPTLC plates and an ethyl acetate–tetrahydrofuran–ammonia mobile phase (10.0 + 7.0 + 0.1, v/v/v). The second method was a reversed-phase HPLC method in which separation was achieved using an acetonitrile–methanol–0.05 M potassium dihydrogen phosphate mobile phase, pH 3.0 (25.0 + 15.0 + 60.0, v/v/v). In both methods, the separated components were detected at 225 nm. Validation of both methods was conducted in compliance with International Conference on Harmonization (ICH) guidelines, and system suitability was confirmed. The linearity ranges were 0.20–28.00 and 0.50–55.00 µg/band for TMC and ECZ by HPTLC, whereas for HPLC, the range was 0.05–30.00 and 1.00–40.00 µg/mL for both drugs, respectively. The methods were successfully applied for the analysis of a pharmaceutical formulation and were compared with the reported method with no significant difference.

Improved liquid-chromatographic determination of haloperidol in plasma.

1984 ◽  
Vol 30 (7) ◽  
pp. 1228-1230 ◽  
Author(s):  
A K Dhar ◽  
H Kutt
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Room Temperature ◽  
Internal Standard ◽  
Isoamyl Alcohol ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract This method for determination of haloperidol in plasma is based on "high-performance" isocratic liquid chromatography with the use of a C8 bonded reversed-phase column at room temperature. Haloperidol and the internal standard (chloro-substituted analog) are extracted from alkalinized plasma into isoamyl alcohol/heptane (1.5/98.5 by vol) and back-extracted into dilute H2SO4. The aqueous phase is directly injected onto the column. The mobile phase is a 30/45/25 (by vol) mixture of phosphate buffer (16.5 mmol/L, pH 7.0), acetonitrile, and methanol. Unlike other liquid-chromatographic procedures for haloperidol, commonly used psychotropic drugs do not interfere. Analysis can be completed within an hour. The procedure is extremely sensitive (1.0 microgram/L) and is well reproducible (CV 5.6% for a 2.5 micrograms/L concentration in plasma).

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