scholarly journals Validation of a Thin-Layer Chromatography for the Determination of Hydrocortisone Acetate and Lidocaine in a Pharmaceutical Preparation

2014 ◽  
Vol 2014 ◽  
pp. 1-10 ◽  
Author(s):  
Małgorzata Dołowy ◽  
Katarzyna Kulpińska-Kucia ◽  
Alina Pyka

A new specific, precise, accurate, and robust TLC-densitometry has been developed for the simultaneous determination of hydrocortisone acetate and lidocaine hydrochloride in combined pharmaceutical formulation. The chromatographic analysis was carried out using a mobile phase consisting of chloroform + acetone + ammonia (25%) in volume composition 8 : 2 : 0.1 and silica gel 60F254plates. Densitometric detection was performed in UV at wavelengths 200 nm and 250 nm, respectively, for lidocaine hydrochloride and hydrocortisone acetate. The validation of the proposed method was performed in terms of specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, and robustness. The applied TLC procedure is linear in hydrocortisone acetate concentration range of3.75÷12.50 μg·spot−1, and from1.00÷2.50 μg·spot−1for lidocaine hydrochloride. The developed method was found to be accurate (the value of the coefficient of variation CV [%] is less than 3%), precise (CV [%] is less than 2%), specific, and robust. LOQ of hydrocortisone acetate is 0.198 μg·spot−1and LOD is 0.066 μg·spot−1. LOQ and LOD values for lidocaine hydrochloride are 0.270 and 0.090 μg·spot−1, respectively. The assay value of both bioactive substances is consistent with the limits recommended by Pharmacopoeia.

Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb

<p><strong>Objective: </strong>A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.</p><p><strong>Methods: </strong>The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F<sub>254</sub> using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.</p><p><strong>Results: </strong>This system was found to have a compact spot of 10-gingerol at <em>R</em><sub>F</sub> value of 0.57±0.03. For the proposed procedure, linearity (<em>r</em><sup>2</sup> = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.</p><p><strong>Conclusion: </strong>Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.</p>


2019 ◽  
Vol 70 (2) ◽  
pp. 487-490
Author(s):  
Nicolae Avram ◽  
Simona Codruta Heghes ◽  
Luca-Liviu Rus ◽  
Anca Maria Juncan ◽  
Lucia Maria Rus ◽  
...  

A HPLC-UV method, for determination of dextromethorphan hydrobromide in syrup, was validated. The chromatographic analysis was performed using an RP-18, Nucleodur chromatographic column (250 mm � 4 mm, 5 �m) at constant temperature (50oC) with a mobile phase consisting of a mixture of acetonitrile/methanol (70:30 v/v) with sodium docusate (as ion pair agent) and ammonium nitrate, pH = 3.4. The flow rate of the mobile phase was 1 mL/min and the detection was carried out at 280 nm. System suitability, specificity, linearity, precision, accuracy, limit of detection and limit of quantification agreed with current pharmacopeial requests. The method is suitable for routine analysis of dextromethorphan hydrobromide in syrup.


2008 ◽  
Vol 5 (4) ◽  
pp. 706-712 ◽  
Author(s):  
A. V. Sulebhavikar ◽  
U. D. Pawar ◽  
K. V. Mangoankar ◽  
N. D. Prabhu-Navelkar

A rapid and simple high performance thin layer chromatography (HPTLC) method with densitometry at λ=263 nm was developed and validated for simultaneous determination of lopinavir and ritonavir from pharmaceutical preparation. Separation was performed on aluminum-backed silica gel 60F254HPTLC plates as stationary phase and using a mobile phase comprising of toluene, ethyl acetate, methanol and glacial acetic acid, in the volume ratio of 7.0:2.0:0.5:0.5 (v/v) respectively. After development, plates were observed under UV light. The detector response was linear in the range of 6.67 to 20.00 µg/spot and 1.67 to 5.00 µg/spot for lopinavir and ritonavir respectively. The validated lowest limit of detection was 21.00 ng/spot and 5.10 ng/spot whereas lowest limit of quantification was 7.00 ng/spot and 21.00 ng/spot for lopinavir and ritonavir respectively. The percentage assay of lopinavir and ritonavir was found between 98.23 to 102.28% and 98.03 to 103.50% respectively. The described method has the advantage of being rapid and easy. Hence it can be applied for routine quality control analysis of lopinavir and ritonavir from pharmaceutical preparation and stability studies.


Chemija ◽  
2021 ◽  
Vol 32 (2) ◽  
Author(s):  
Yuliia Maslii ◽  
Ivan Bezruk ◽  
Anna Materiienko ◽  
Olena Ruban ◽  
Liudas Ivanauskas ◽  
...  

A new high-performance liquid chromatography (HPLC) method for the simultaneous quantitative determination of active pharmaceutical substances and preservatives in a new dental medication has been developed. The optimization of HPLC method parameters was done through studies of a mobile phase composition and a detection wavelength. Our developing method uses an ACE C18 column (250 × 4.6 mm, 5 µm) and a gradient mode for separation with the acetonitrile and phosphate buffer solution (adjusted to pH 3.0) as mobile phases. The flow rate is 1 ml/ min, and the detection was set at 260 nm (DAD). The method was evaluated according to the ICH guidelines and the State Pharmacopoeia of Ukraine in terms of specificity, accuracy, linearity and precision (repeatability and intermediate precision). The limit of detection and the limit of quantification were also calculated. The developed method was put in place for the analysis of a combined dental gel to a quantitative determination of the APIs (choline salicylate, lidocaine hydrochloride) and preservatives (methylparaben, propylparaben).


2020 ◽  
Vol 11 (4) ◽  
pp. 291-297
Author(s):  
Hutaf Mustafa Baker ◽  
Hussam Ahmad Alsaoud ◽  
Hamzeh Mohamad Abdel-Halim

A simple, sensitive and reproducible method for the determination of ranitidine hydrochloride in pharmaceutical preparations was investigated. This spectrophotometric method was based on the formation of a deep red color product with ninhydrin in basic media and the absorbance measured at λmax = 480 nm. The reaction occurs at 45 °C with pH = 10 having a contact time of 38 minutes. Under the optimum conditions, Beer’s Law is obeyed in the concentration range of 8.98×103 - 9.90×104 µg/L. The coefficient of correlation was found to be 0.999 for the obtained method with molar absorptivity of 3.05×103 L/mol.cm. The calculated Sandell’s sensitivity is 0.108 μg/cm2. The limit of detection and limit of quantification are 0.0997 and 0.3023 µg/mL, respectively. The low values of the percentage relative standard deviation and percentage relative error indicate the high precision and the good accuracy of the proposed method. The stoichiometry of the reaction is determined and found to be 1:4 (Ranitidine hydrochloride:Ninhydrin). The initial rate method confirmed that this reaction is first order one.


Author(s):  
Ankita Gaikwad ◽  
Madhuri Shelar ◽  
Ganesh Andhale ◽  
Jyoti Kadam

Resveratrol is a plant compound that work as antioxidant and it also has anti-aging properties whereas Piperine is a alkaloid and it majorly used in spices.  A HPTLC (High performance thin layer chromatography) study is conducted for estimation of Resveratrol and Piperine. The Mobile phase used was Chloroform: Ethyl Acetate (50:50 v/v). Rf Value of Resveratrol 0.59 and Piperine 0.79 was found. Stationary phase of Silica gel 60 F254 was used. Densitometric analysis was performed at 325 nm. The method was found to be linear. Recovery (ranging from 97% to 102.24 %), limit of detection (40.26 ng/spot, 1.64 ng/spot respectively for resveratrol & piperine), limit of quantification (122.02 ng/spot, 4.98 ng/spot respectively for resveratrol & piperine) and precision (≤ 2.00%) were found to be satisfactory. Validation performed with linearity, accuracy, precision, specificity, robustness, limit of detection and limit of quantification. Every parameter found within the range. The developed method allows to confirm that an accurate and reliable potency measurement of a pharmaceutical preparation can be performed.


2012 ◽  
Vol 2 (1) ◽  
pp. 7-10 ◽  
Author(s):  
Nia Kristiningrum ◽  
Mia Rakhmawati

A rapid and reproducible TLC method was developed for the determination of hydrocortisone acetate and chloramphenicol in cream. The analytes were dissolved with methanol and chromatographed on silica Gel GF 254 TLC plate using chloroform:ethyl acetate in the ratio of 1:1.5 (v/v) as mobile phase. Spots at Rf 0.29 and Rf 0.59 were recognized as chloramphenicol and hydrocortisone acetate, respectively. Quantitative analysis was done through densitometric measurement at wavelength 265 nm. Method was found linear over the concentration range of 300-900 ng/spot with the correlation coefficient of 0.999 and 0.998 for hydrocortisone acetate and chloramphenicol, respectively. Specificity showed calculation of purity and identity more than 0.99. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were 23.84 and 71.51 ng/spot for hydrocortisone acetate, 21.06 and 63.18 ng/spot for chloramphenicol. The precision of this method was less than 2.8% whereas the means of the recovery data were 100.40± 0.579% for hydrocortisone acetate and 100.24±1.20% for chloramphenicol. The proposed method has been applied to the determination of hydrocortisone acetate and chloramphenicol in commercial cream formulations and the recovery of label claim were 99.23±0.66% (chloramphenicol) and 99.25±0.41% (hydrocortisone acetate) for brand A and 100.32±0.87% (chloramphenicol) and 100.53±0.78% (hydrocortisone acetate) for brand B. The developed method was successfully used for the assay of hydrocortisone acetate and chloramphenicol. The method is simple, sensitive and precise; it can be used for the routine quality control testing of marketed formulations.DOI: http://dx.doi.org/10.3329/icpj.v2i1.12871 International Current Pharmaceutical Journal 2012, 2(1): 7-10 


Author(s):  
Mohammad Mojeeb Gulzar Khan ◽  
Pawar Vivek Laxman ◽  
Abdul Talib ◽  
Sandip Dinkar Firke ◽  
Mohan G Kalaskar ◽  
...  

For the determination of pimvanserin tartrate in bulk and formulation, a rapid and simple High Performance Thin Layer Chromatography at 226 nm was developed and validated. The determination was carried out on thin coated aluminum backing plates covered with 200 mm layer of silica gel G 60 F254 (10×10 cm) plate as stationary phase and using a mobile phase of methanol: chloroform: trimethylamine (4:6:0.1 v/v/v) respectively. With a correlation coefficient (r) of 0.998, the development of pimvanserin tartrate was linear in the range of 0.7 to 4.2 µg/ml. The limit of detection (LOD) was found to be 7.68 ng/spot while the limit of quantification was found to be 23.28 ng/spot. The percentage label claim of pimvanserin tartrate in bulk and formulation was found to be 99 – 101 %. The percentage found in the formulation shows that no effect of excipient on drug. The conducted procedure has the benefit of being simple and quick. As a result, it can be used to examine pimvanserin tartrate in pharmaceutical formulations.


2019 ◽  
Vol 10 (2) ◽  
pp. 1367-1371
Author(s):  
Khalaf F Al Samarrai ◽  
Eman Thiab A Al Samarrai ◽  
Baidaa Adnan Al Samarrai

A simple, rapid and low-cost spectrophotometric method for determination of Methyldopa (MDA) based on ion-pair formation using Bromothymol blue (BTB) as a reagent in alkaline medium (pH 8.7). The absorbance of the green-blue-coloured product is measured at 616 nm. Beer's Law is obeyed at concentration range up to 5-20μg/ml with molar absorptivity 0.8279x104 L/mol.cm. The correlation coefficient, limit of detection and limit of quantification were 0.9982, 0.4318 μg/ml and 1.4393 μg/ml respectively. The method has been successfully applied to the determination of Methyldopa in pharmaceutical preparations.


Author(s):  
Mohammad Hamzah Hamzah ◽  
Rawa M M Taqi ◽  
Muna M. Hasan ◽  
Raid J. M. Al-Timimi

A simple and accurate spectrophotometric method for the determination of Trifluoperazine HCl in pure and dosage forms was developed. The method is based on the reaction between Trifluoperazine HCl and p-chloroaniline in the presence of cerium ion as oxidizing agent which lead to the formation of violate color product that absorbed at a maximum wavelength 570nm while the blank solution was pink. Under the optimum conditions a linear relationship between the intensity and concentration of TRF in the range 4-50μg/ml was obtained . The molar absorptivity 3.74×103 L.mol-1.cm-1 , Limit of detection (2.21μg/ml), while limit of quantification was 7.39μg/ml. The proposed analytical method was compared with standard method using t-test and F-test , the obtained results shows there is no significant differences between proposed method and standard method. Based on that the proposed method can be used as an alternative method for the determination of TRF in pure and dosage forms.


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