scholarly journals Influence of Different Chromatographic Conditions on the Level of Detection and Quantitation of Spironolactone by means of TLC-Densitometry

2019 ◽  
Vol 2019 ◽  
pp. 1-8 ◽  
Author(s):  
Małgorzata Dołowy
Keyword(s):  
Quality Control ◽  
Acetic Acid ◽  
Ethyl Acetate ◽  
Mobile Phase ◽  
Glacial Acetic Acid ◽  
Cost Effective ◽  
Pharmaceutical Formulations ◽  
The One ◽  
Tlc Analysis ◽  
Routine Quality Control

The aim of this study was to estimate the influence of different chromatographic conditions on the limits of detection and limits of quantitation (LODs and LOQs) of spironolactone by means of TLC-densitometry under different chromatographic conditions. A comparison of results obtained showed that the choice of appropriate chromatographic conditions for NP-TLC and RP-TLC analysis with densitometry could effectively decrease the LODs and LOQs of spironolactone. Of all chromatographic systems tested, the best was the one comprising chromatographic plates precoated with a mixture of silica gel 60, kieselguhr F254, and mobile phase A (n-hexane-ethyl acetate-glacial acetic acid, 24.5 : 24.5 : 1, v/v/v). The estimated average LOD and LOQ values were 0.034 and 0.103 μg/spot, respectively. This indicates that the described procedure is sufficiently sensitive for the identification and quantification of spironolactone alone. Thereby, the simple and cost-effective TLC-densitometric method can be utilized for the routine quality control of spironolactone in bulk drugs as well as in simple pharmaceutical formulations.

Validated HPTLC Method for the Estimation of Oxetacaine in Pharmaceutical Formulations

2021 ◽  
pp. 5668-5672
Author(s):  
Kavitha J ◽  
Bonda Vismitha ◽  
Kokilambigai KS ◽  
Seetharaman R ◽  
Lakshmi KS
Keyword(s):  
Mobile Phase ◽  
Glacial Acetic Acid ◽  
Current Method ◽  
Cost Effective ◽  
Pharmaceutical Formulations ◽  
Relieve Pain ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Chromatographic Resolution ◽  
Hptlc Method

Oxetacaine is a potent local anesthetics used to relieve pain associated with peptic ulcer. The current method details about a rapid, accurate and precise HPTLC technique for the assessment of Oxetacaine in Pharmaceutical formulation. Chromatographic resolution was carried out on precoated HPTLC plates (Silica gel 60 F254 on Aluminum plate) employing methanol: water: glacial acetic acid (8: 1.8: 0.2 v/v/v) as mobile phase. Densitometric assessment was carried out at 220nm [Camag TLC Scanner III with winCATs software (version – 1.3.4)]. The drug was identified with a Rf value of 0.61. The reliability of the projected method was ascertained by evaluating various validation parameters as per ICH guidelines. The proposed technique can evaluate ten or more formulation units concurrently in a single run and affords a more rapid and cost-effective QC tool for regular analysis of Oxetacaine in pharmaceutical formulations.

Comparative Study for Selection of the Optimum Mobile Phase for Separation of Caffeine and Paracetamol by Using TLC Chromatographic Method

2017 ◽  
Vol 8 (1) ◽  
Author(s):  
Mohammed Gamal ◽  
Ali Turki ◽  
Almonzer Al-Shemari ◽  
Abd Alla Alomari
Keyword(s):  
Acetic Acid ◽  
Literature Review ◽  
Comparative Study ◽  
Ethyl Acetate ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Glacial Acetic Acid ◽  
Mobile Phases ◽  
Selection Of

Objective. To investigate the best mobile phase for separation of Paracetamol (PAR) and Caffeine (CAF) using TLC method. Methods. Different mobile phases which were mentioned in literature review were tried and retention times for both PAR and CAF were recorded for each experiment separately. Results : It was found that retardation factors for solvent A Rf (PAR) =0,59 and Rf(CAF)=0,90 ; for solvent B Rf(PAR)=0,92 and Rf(CAF)=0,81; Rf(PAR)=0,22 and Rf (CAF)=0,16. Solvent A is composed of n-hexane-ethyl acetate-ethanol (2.5 + 1.5 + 0.4, v/v/v), solvent B is composed of chloroform,ethyl acetate and ammonia (15,0 + 4,3 + 0,3 v/v/v) and solvent C is composed of methanol,glacial acetic acid and water (25,0 +4,3+70,7 v/v/v ). Conclusion: It was found that the best solvent for separation of CAF and PAR in TLC chromatographic method was composed of n-hexane-ethyl acetate-ethanol (2.5 + 1.5 + 0.4, v/v/v).

HSCCC Separation of Three Main Compounds from the Crude Extract of Dracocephalum Tanguticum by Using Dimethyl Sulfoxide as Cosolvent

2020 ◽  
Author(s):  
Xue Yang ◽  
Yongling Liu ◽  
Tao Chen ◽  
Nana Wang ◽  
Hongmei Li ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Ethyl Acetate ◽  
Dimethyl Sulfoxide ◽  
Efficient Method ◽  
Crude Extract ◽  
High Speed ◽  
Glacial Acetic Acid ◽  
Butyl Alcohol ◽  
Preparative Hplc ◽  
Counter Current

Abstract Separation of natural compounds directly from the crude extract is a challenging work for traditional column chromatography. In the present study, an efficient method for separation of three main compounds from the crude extract of Dracocephalum tanguticum has been successfully established by high-speed counter-current chromatography (HSCCC). The crude extract was directly introduced into HSCCC by using dimethyl sulfoxide as cosolvent. Ethyl acetate/n-butyl alcohol/0.3% glacial acetic acid (4: 1: 5, v/v) system was used and three target compounds with purity higher than 80% were obtained. Preparative HPLC was used for further purification and three target compounds with purity higher than 98% were obtained. The compounds were identified as chlorogenic acid, pedaliin and pedaliin-6″-acetate.

DEVELOPMENT OF HPTLC METHOD FOR SIMULTANEOUS ESTIMATION OF CIPROFLOXACIN AND ORNIDAZOLE IN COMBINED DOSAGE FORM

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (05) ◽  
pp. 36-43
Author(s):  
N. R Dighade ◽  
◽  
M. D Shende ◽  
A. V Kasture
Keyword(s):  
Quality Control ◽  
High Resolution ◽  
Thin Layer ◽  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Simultaneous Estimation ◽  
Ich Guidelines ◽  
Hptlc Method ◽  
Routine Quality Control

A simple and accurate high performance thin layer chromatographic (HPLTC) method has been developed and validated as per ICH guidelines for estimations of Ciprofloxacin (CP) and Ornidazole (ORN) in combined dosage form. The mobile phase was acetonitrile: toluene: water and triethylamine (5.5:1.8:1.5:1.6 V/V) was found to be best which gave high resolution with Rf 0.16 and 0.84 for ciprofloxacin and ornidazole respectively. The linearity of ciprofloxacin and ornidazole was found to be in the range of 0.4 to 0.8 µg/mL and 0.4 to 0.8 µg/mL, respectively. The coefficient of correlation (r2 ) was found to be greater than 0.989 for both the components by this method. The tablet analyses result (n = 5) were found to be > 100.84 % by HPTLC for both the components. The proposed method was found to be simple, accurate and suitable for routine quality control of marketed formulations containing these drugs.

scholarly journals Thin layer chromatographic compatibility study in preformulation of new transdermal therapeutic systems

2020 ◽  
Vol 66 (1) ◽  
pp. 23-29
Author(s):  
Octavia-Laura Moldovan ◽  
Diana-Nicoleta Brihan ◽  
Nicoleta Todoran ◽  
Aura Rusu
Keyword(s):  
Acetic Acid ◽  
Thin Layer ◽  
Mobile Phase ◽  
Glacial Acetic Acid ◽  
Methylene Chloride ◽  
Hydroxyethyl Cellulose ◽  
Compatibility Study ◽  
Chemical Interactions ◽  
Miconazole Nitrate ◽  
Active Substances

AbstractObjective: The compatibility of four binary active substances combinations adapalene – levofloxacin (ADP-LFX), adapalene – miconazole nitrate (ADP-MCZ), levofloxacin – meloxicam (LFX-MLX) and levofloxacin – miconazole nitrate (LFX-MCZ) was analysed to be comprised in new transdermal therapeutic systems. Also, the compatibility of selected active substances and four polymeric excipients (hydroxypropyl methyl-cellulose - HPMC 15000, hydroxypropyl methylcellulose - HPMC E5, ethyl cellulose - EC 10, and hydroxyethyl cellulose – HEC) was studied.Methods: Thin layer chromatographic method (TLC) and four selected mobile phases were used. On the plate (in situ) were obtained the binary combinations (active substances and active substance-polymer).Results: A good compatibility of ADP-LFX was found using ammonia : methanol : acetonitrile : methylene chloride 2:4:1:4 mobile phase. Using chloroform : acetone : glacial acetic acid 34:4:3 on the chromatogram of ADP-MCZ, only ADP spots appeared but without changes in the shape of the spots and Rf values. Any modifications of LFX and MLX spots (from LFX-MLX mixture) had been observed using toluene : glacial acetic acid : methanol 11:1:0.5 mobile phase, although LFX spots have remained on the baseline. Only LFX spots were visible from LFX-MLX and LFX-MCZ mixtures (ammonia : methanol : acetonitrile : methylene chloride 2:4:1:4 mobile phase). Distinctive spots were observed for ADP, LFX and MLX with variable results from no chemical interactions to limited chemical interactions when the compatibility with polymers was verified.Conclusions: ADP-LFX and LFX-MLX mixtures were found to be compatible. ADP with HPMC polymers and LFX with HPMC E5 and HEC had presented excellent compatibility; for the other binary combinations, different analytical methods will be necessary.

scholarly journals Spectrodensitometric simultaneous determination of esomeprazole and domperidone in human plasma

2017 ◽  
Vol 15 (1) ◽  
pp. 293-298
Author(s):  
Pakinaz Y. Khashaba ◽  
Hassan Refat H. Ali ◽  
Mohamed M. El-Wekil
Keyword(s):  
Ethyl Acetate ◽  
Factorial Design ◽  
Simultaneous Determination ◽  
Human Plasma ◽  
Mobile Phase ◽  
Fractional Factorial Design ◽  
Cost Effective ◽  
Fractional Factorial ◽  
Tlc Plates

AbstractA simple, rapid, cost-effective, and sensitive TLC-spectrodensitometric method for simultaneous determination of esomeprazole and domperidone was developed and tested in human plasma. Ethyl acetate: methanol: benzene: acetonitrile (5: 4: 8: 3, v/v/v/v) mobile phase was used for separation on TLC plates detected at 286 nm. The linearity ranges were 5-1200 and 2-600 ng/ spot for esomeprazole and domperidone, and limits of detection were 1.73 and 0.59 ng/spot. The effects of four variables affecting Rf were evaluated by fractional factorial design. The benzene volume and saturation time had significant effects.

scholarly journals Determination of Delafloxacin in Pharmaceutical Formulations Using a Green RP-HPTLC and NP-HPTLC Methods: A Comparative Study

Antibiotics ◽  
2020 ◽  
Vol 9 (6) ◽  
pp. 359 ◽  
Author(s):  
Prawez Alam ◽  
Essam Ezzeldin ◽  
Muzaffar Iqbal ◽  
Gamal A.E. Mostafa ◽  
Md. Khalid Anwer ◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
Silica Gel ◽  
Solid Lipid Nanoparticles ◽  
Ternary Mixture ◽  
Mobile Phase ◽  
Pharmaceutical Formulations ◽  
Lipid Nanoparticles ◽  
Ammonia Solution ◽  
Hptlc Method

In this work; delafloxacin (DLFX) was determined using a validated green RP-HPTLC and NP-HPTLC methods in commercial tablets and in-house developed solid lipid nanoparticles (SLNs). RP-HPTLC determination of DLFX was performed using “RP-18 silica gel 60 F254S HPTLC plates”. However; NP-HPTLC estimation of DLFX was performed using “silica gel 60 F254S HPTLC plates”. For a green RP-HPTLC method; the ternary combination of ethanol:water:ammonia solution (5:4:2 v/v/v) was used as green mobile phase. However; for NP-HPTLC method; the ternary mixture of ethyl acetate: methanol: ammonia solution (5:4:2 v/v/v) was used as normal mobile phase. The analysis of DLFX was conducted in absorbance/reflectance mode of densitometry at λmax = 295 nm for both methods. RP-HPTLC method was found more accurate, precise, robust and sensitive for the analysis of DLFX compared with the NP-HPTLC method. The % assay of DLFX in commercial tablets and in-house developed SLNs was determined as 98.2 and 101.0%, respectively, using the green RP-HPTLC technique, however; the % assay of DLFX in commercial tablets and in-house developed SLNs was found to be 94.4 and 95.0%, respectively, using the NP-HPTLC method. Overall, the green RP-HPTLC method was found superior over the NP-HPTLC. Therefore, the proposed green RP-HPTLC method can be successfully applied for analysis of DLFX in commercial tablets, SLNs and other formulations containing DLFX.

scholarly journals Production of Indole-3-Acetic Acid: A White Biotechnology for Weed Biocontrol

2021 ◽  
Author(s):  
Sakaoduoen Bunsangiam ◽  
Nutnaree Thongpae ◽  
Savitree Limtong ◽  
Nantana Sri
Keyword(s):  
Acetic Acid ◽  
Cost Effective ◽  
Pilot Scale ◽  
Cyperus Rotundus ◽  
Shake Flask Culture ◽  
Iaa Production ◽  
Weed Growth ◽  
Fold Reduction ◽  
The One ◽  
Indole 3 Acetic Acid

Abstract Indole-3-acetic acid (IAA) is the most common plant hormone of the auxin class and regulates various plant growth processes. The present study investigated IAA production by the basidiomycetous yeast Rhodosporidiobolus fluvialis DMKU-CP293 using the one-factor-at-a-time (OFAT) method and response surface methodology (RSM). IAA production was optimized in shake-flask culture using a cost-effective medium containing 4.5% crude glycerol, 2% CSL and 0.55% feed-grade L-tryptophan. The optimized medium resulted in a 3.3-fold improvement in IAA production and a 3.6-fold reduction in cost compared with those obtained with a non-optimized medium. Production was then scaled up to a 15-L bioreactor and to a pilot-scale (100-L) bioreactor based on the constant impeller tip speed (Vtip) strategy. By doing so, IAA was successfully produced at a concentration of 3,569.32 mg/L at the pilot scale. To the best of our knowledge, this is the first report of pilot-scale IAA production by microorganisms. In addition, we evaluated the effect of crude IAA on weed growth. The results showed that weed (Cyperus rotundus L.) growth could be inhibited by 50 mg/L of crude IAA. IAA therefore has the potential to be developed as a herbicidal bioproduct to replace the chemical herbicides that have been banned in various countries, including Thailand.

scholarly journals Techno-Economic Analysis of Producing Glacial Acetic Acid from Poplar Biomass via Bioconversion

Molecules ◽  
2020 ◽  
Vol 25 (18) ◽  
pp. 4328
Author(s):  
Rodrigo Morales-Vera ◽  
Jordan Crawford ◽  
Chang Dou ◽  
Renata Bura ◽  
Rick Gustafson
Keyword(s):  
Acetic Acid ◽  
Enzymatic Hydrolysis ◽  
Economic Analysis ◽  
Ethyl Acetate ◽  
Glacial Acetic Acid ◽  
Commercial Production ◽  
Economic Feasibility ◽  
Distillation Columns ◽  
Capital Costs ◽  
Economical Process

Most of the current commercial production of glacial acetic acid (GAA) is by petrochemical routes, primarily methanol carbonylation. GAA is an intermediate in the production of plastics, textiles, dyes, and paints. GAA production from biomass might be an economically viable and sustainable alternative to petroleum-derived routes. Separation of acetic acid from water is a major expense and requires considerable energy. This study evaluates and compares the technical and economic feasibility of GAA production via bioconversion using either ethyl acetate or alamine in diisobutylkerosene (DIBK) as organic solvents for purification. Models of a GAA biorefinery with a production of 120,650 tons/year were simulated in Aspen software. This biorefinery follows the path of pretreatment, enzymatic hydrolysis, acetogen fermentation, and acid purification. Estimated capital costs for different scenarios ranged from USD 186 to 245 million. Recovery of GGA using alamine/DIBK was a more economical process and consumed 64% less energy, due to lower steam demand in the recovery distillation columns. The estimated average minimum selling prices of GGA were USD 756 and 877/ton for alamine/DIBK and ethyl acetate scenarios, respectively. This work establishes a feasible and sustainable approach to produce GGA from poplar biomass via fermentation.

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