scholarly journals Stability-Indicating Photochemical Method for the Assay of Thiamine by Spectrophotometry

2018 ◽  
Vol 2018 ◽  
pp. 1-7 ◽  
Author(s):  
Iqbal Ahmad ◽  
Syed Haider Abbas ◽  
Zubair Anwar ◽  
Muhammad Ali Sheraz ◽  
Sofia Ahmed ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
The United States ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Low Concentrations ◽  
Photochemical Method ◽  
Significant Difference ◽  
Liquid Chromatography Method ◽  
States Pharmacopeia

A stability-indicating photochemical method has been developed for the assay of thiamine (TH) salts in aqueous solution and in fresh and aged vitamin preparations. It is based on the photooxidation of TH by UV irradiation to form thiochrome (TC) in alkaline solution. The TC : TH ratio under controlled conditions of light intensity, temperature, pH, exposure time, and irradiation distance is constant and can be used to determine the concentration of UV irradiated TH solutions. TC, on extraction with isobutanol from the photodegraded solution of TH, has been determined by the UV spectrophotometric method at 370 nm. It exhibits a high intensity of absorption in the UV region that can be used for the assay of even low concentrations of TH. Under optimum conditions, Beer’s law is obeyed in the concentration range of 0.20–2.00 mg/100 ml (R2 = 09998). The limit of detection (LOD) and limit of quantification (LOQ) are 0.0076 and 0.0231 mg/100 ml, respectively. The method has been validated and applied to aqueous solutions and vitamin preparations. The results have statistically been compared with the United States Pharmacopeia liquid chromatography method. It has been found that there is no significant difference between the two methods at 95% confidence level.

scholarly journals Oxytetracycline Residues in Honey Analyzed by Liquid Chromatography with UV Detection

2013 ◽  
Vol 57 (1) ◽  
pp. 25-32 ◽  
Author(s):  
Anna Gajda ◽  
Andrzej Posyniak ◽  
Andrzej Bober ◽  
Tomasz Błądek ◽  
Jan Żmudzki
Keyword(s):  
Liquid Chromatography ◽  
Oxalic Acid ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Experimental Treatment ◽  
Uv Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method

Summary A liquid chromatography method with UV detection for determination of oxytetracycline (OTC) in honey has been developed. The samples were extracted with the solution of oxalic acid. The clean-up procedure was performed by solid phase extraction (SPE) using polymeric Strata X and carboxylic acid cartridges. Chromatographic separation was carried out on the Luna C8 analytical column with mobile phase consisting of acetonitrile-0.02 M oxalic acid. The method has been successfully validated according to the requirements of the European Decision 2002/657/EC and this method is used in routine control of oxytetracycline in honey samples. The limit of detection (LOD) and limit of quantification (LOQ) of the presented method were 10 and 12.5 μg/kg, respectively. The developed method has also been verified in quantitative determination of oxytetracycline residues in honey after experimental treatment with this product in bee colonies.

scholarly journals Simultaneous Estimation and Validation of Atorvastatin Calcium and Aspirin in Combined Capsule Dosage Form by RP HPLC Method

2012 ◽  
Vol 9 (3) ◽  
pp. 1449-1456
Author(s):  
B. V. Suma ◽  
K. Kannan ◽  
V. Madhavan ◽  
Chandini R. Nayar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Atorvastatin Calcium ◽  
Ich Guidelines ◽  
Phase Liquid ◽  
Liquid Chromatography Method

A new simple, specific, precise and accurate revere phase liquid chromatography method has been developed for estimation of atorvastatin calcium (AST) and ASPIRIN (ASP) simultaneously in a combined capsule dosage forms. The chromatographic separation was achieved on a 5 – micron C 18 column (250x 4.6mm) using a mobile phase consisting of a mixture of Acetonitrile: Ammonium Acetate buffer 0.02M (68:32) pH 4.5. The flow rate was maintained at 0.8 ml/min. The detection of the constituents was done using UV detector at 245 nm for AST and ASP. The retention time of AST and ASP were found be 4.5915 ± 0.0031 min and 3.282 ±0.0024 min respectively. The developed method was validated for accuracy, linearity, precision, limit of detection (LOD) and limit of quantification (LOQ) and robustness as per the ICH guidelines.

scholarly journals Determination of Formaldehyde by HPLC with Stable Precolumn Derivatization in Egyptian Dairy Products

2018 ◽  
Vol 2018 ◽  
pp. 1-5 ◽  
Author(s):  
Ahmed Salem Sebaei ◽  
Ahmed M. Gomaa ◽  
A. A. El-Zwahry ◽  
E. A. Emara
Keyword(s):  
Dairy Products ◽  
High Performance ◽  
Limit Of Detection ◽  
Precolumn Derivatization ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Derivatizing Agent ◽  
Array Detection ◽  
Liquid Chromatography Method

Formaldehyde is one of the most dangerous chemical compounds affecting the human health; exposure to it from food may occur naturally or by intentional addition. In this study a high performance liquid chromatography method for determination of formaldehyde in dairy products was described. The dairy samples were reacted and extracted with a warmed organic solvent in the presence of derivatizing agent 2,4-dinitrophenylhydrazine (DNPH) and formaldehyde; the mixture was centrifuged and followed by diode array detection. The method is validated and gives average recovery of formaldehyde at the three different levels 0.1, 5.0, and 10.0 mg/kg varied between 89% and 96%. The method is linear from the limit of quantification 0.1 mg/kg up to 10 mg/kg levels. This method is intended for formaldehyde analyses in dairy products simply with stable derivatization, minimum residue loss, excellent recovery, and accurate results with a sensitive limit of detection 0.01 mg/kg. 90 dairy samples from milk, cheese, and yogurt were investigated from seven Egyptian governorates and all samples were free from formaldehyde.

scholarly journals Validated Stability Indicating HPLC Method for Simultaneous Quantification of Trithioparamethoxy Phenylpropene and Chlorpheniramine Maleate in Tablet Forms

2020 ◽  
Vol 32 (6) ◽  
pp. 1291-1296
Author(s):  
T. Sravanthi ◽  
N. Madhavi
Keyword(s):  
High Performance ◽  
Hplc Method ◽  
Base Hydrolysis ◽  
Chlorpheniramine Maleate ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Liquid Chromatography Method ◽  
Concurrent Assessment ◽  
Oxidation Degradation

A novel easy stability indicating high performance liquid chromatography method has been developed for the concurrent assessment of trithioparamethoxy phenylpropene in combination with chlorpheniramine maleate using Luna C8 column with UV detection at 224 nm. The mobile phase comprised of 0.02 N phosphate buffer (pH 5.5) and acetonitrile (55:45 v/v) was delivered with a flow rate of 1.5 mL/min. The method was linear over the concentration range 6.25-18.75 μg/mL (trithioparamethoxy phenylpropene) and 1.5-4.5 μg/mL (chlorpheniramine maleate). The limit of quantification was 1.57 μg/mL (trithioparamethoxy phenylpropene) and 0.969 μg/mL (chlorpheniramine maleate). The calculated recoveries were 100.083-100.287% (trithioparamethoxy phenylpropene) and 99.827-100.277% (chlorpheniramine maleate). Trithioparamethoxy phenylpropene and chlorpheniramine maleate were subjected to forced stress like acid hydrolysis, base hydrolysis, thermal and oxidation degradation. The drugs were found to degrade in the applied conditions. The degraded products were resolved effectively from the trithioparamethoxy phenylpropene and chlorpheniramine maleate. The suggested stability-indicating HPLC method can be used for the quantitative evaluation of trithioparamethoxy phenylpropene and chlorpheniramine maleate in bulk medications and tablet formulations.

scholarly journals Research Article on Development and Validation of RP-HPLC Method for Estimation of Canagliflozin

2019 ◽  
Vol 11 (02) ◽  
pp. 85-92
Author(s):  
Gudipally. Mounika ◽  
K. Bhavya Sri ◽  
R. Swethasri ◽  
M. Sumakanth
Keyword(s):  
Retention Time ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Validation Parameters ◽  
Liquid Chromatography Method ◽  
Development And Validation

To develop an accurate, precise, specific high performance liquid chromatography method for quantification of Canagliflozin in bulk and dosage forms. A C18 column (250mm X 4.6mm; 5μm phenomenex) was used with mobile phase containing Acetonitrile-0.1% sodium acetate buffer (pH-4.6), (20:80) in isocratic mode. The flow rate maintained was 1.0ml/min and the U.V detector was operated at 291nm. The retention time of Canagliflozin was 3.307min and showed a good linearity in concentration range of 2-14μg/ml with correlation coefficient of 0.999. The average percent recovery was found to be 99.98%. The developed method follows validation parameters such as system suitability, linearity, precision, accuracy, limit of detection and limit of quantification and robustness as per ICH guidelinesQ2(R1). The proposed method was found to provide faster retention time with sharp resolution with linearity at a lowest concentration as compared to previous methods and this method is validated as per International conference on harmonization guidelines and successfully applied for bulk and pharmaceutical dosage form.

RAPID HIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE DETERMINATION OF RALTEGRAVIR IN HUMAN SALIVA

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (09) ◽  
pp. 68-73
Author(s):  
K Vijaya Sri ◽  
M. Shiva Kumar ◽  
M. A. Madhuri ◽  
Suresha K. ◽  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Human Saliva ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method ◽  
Liquid Chromatographic

In this study, a high-performance liquid chromatographic method (HPLC) was developed, validated and applied for the determination of raltegravir in biological sample like saliva. Liquid- liquid extraction was performed for isolation of the drug and elimination of saliva interferences. Samples of saliva was extracted with 50µL of ortho phosphoric acid and 3ml of methanol was added and spiked with raltegravir. The chromatographic separation was performed on Agilent Eclipse C18 (100 mm × 4.6 mm, 3.5µm) column, by using 80:20 v/v acetonitrile: water as a mobile phase under isocratic conditions at a flow rate of 1.0 mL/min for UV detection at 240 nm. Retention time of raltegravir was found to be 1.030 min. Linearity was found to be in the range of 25-1000 ng/mL with regression equation y = 13864x + 40495 and correlation coefficient 0.999. The low % RSD value indicates the method is accurate and precise. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.76 and 2.28 ng/mL, respectively. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for determination of raltegravir in saliva.

Simultaneous Estimation of Apremilast and Betamethasone Dipropionate in Microsponge-Based Topical Formulation using a Stability Indicating RP-HPLC Method: A Quality-by-Design Approach

2021 ◽  
Author(s):  
Prashansha Mullick ◽  
Sadhana P Mutalik ◽  
Aswathi R Hegde ◽  
Abhijeet Pandey ◽  
P C Jagadish ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Betamethasone Dipropionate ◽  
Simultaneous Estimation ◽  
Topical Formulation ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Column Temperature ◽  
Stability Indicating ◽  
Relative Standard

Abstract A stability-indicating reverse phase high-performance liquid chromatography method was developed and validated for simultaneous quantification of apremilast (APL) and betamethasone dipropionate (BD) in bulk as well as drug loaded microsponges. Various mobile phase systems were screened to check the system suitability followed by force degradation analysis to determine APL and BD stability under varying stress conditions. A central composite design model was used to optimize the column temperature and flow rate using Design Expert® (9.0.1). One factor at a time approach with five independent factors were used to validate the robustness of the method. Finally, APL and BD were precisely and accurately quantified from drug loaded microsponges using the validated method. A favorable separation of APL and BD was obtained on a Phenomenex® Luna C18 column using a mixture of 50 mM phosphate buffer containing 0.1% triethylamine (pH 6.1) and acetonitrile (60:40%v/v) as mobile phase. Both the drugs were found to be stable when exposed to stressors such as heat-, light-, alkali-, acid- and peroxide-induced degradation. The calibration curves were found to be linear with appreciable limit of detection and limit of quantification. Recovery and percentage relative standard deviation of peak areas for APL and BD were found to be < 2.0% and 99–100% in bulk drug solution and <2.0% and 99–103% in microsponge formulation, respectively. Statistical analysis using analysis of variance indicated that the model was significant (P < 0.001). Hence, the developed method can be effectively used to quantify APL and BD, both in bulk as well as microsponge formulations.

Development of Validated Stability Indicating HPTLC Method for the Estimation of Teriflunomide in Bulk and Tablet Dosage Form

2020 ◽  
Vol 16 (7) ◽  
pp. 814-822
Author(s):  
Snehal Karmankar ◽  
M. Tajne
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Immunosuppressive Agents ◽  
Pharmaceutical Preparations ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Tablet Dosage

Background: Teriflunomide is an immunosuppressive agent. Immunosuppressive agents are drugs that inhibit or prevent activity of immune system. Teriflunomide was investigated as a medication for multiple sclerosis (MS). Various studies have reported the HPLC, UPLC, LC/MS methods for the estimation of teriflunomide. However, till date stability indicating HPTLC analysis method has not been reported for the estimation of teriflunomide in bulk and tablet dosage form. Objective: Objective of the present work was to develop and validate stability indicating high performance thin layer chromatography method for the determination of teriflunomide in bulk and tablet dosage form. Methods: Chromatography was performed on aluminium plates coated with silica gel 60F254 using toluene, methanol and acetic acid (7.5: 2.5: 0.05 v/v/v) as mobile phase. Densitometric analysis was performed at 254 nm. The method was validated with different parameters such as linearity, precision, accuracy, specificity, robustness, limit of detection (LOD) and limit of quantitation (LOQ). The RF value of teriflunomide was 0.56 ± 0.03. The method is sensitive (limit of quantification 17.83 ng/band), precise (RSD ≤ 1.34%), accurate (drug recovery 98.49–99.53 %), and linear over the range 100–600 ng/band (r2 0.998). Results: Degradation products were found in stress conditions did not interfere with the detection of teriflunomide; therefore, the proposed technique can be considered stability-indicating. Teriflunomide did not degrade under alkaline hydrolysis, thermal and photolytic conditions but showed degradation under acid hydrolysis and oxidation with about 14.5 and 13.8 % decompositions respectively. Conclusion: The developed method was satisfactorily applied for the analysis of pharmaceutical preparations and proved to be specific and accurate for quality control of the cited drugs in their tablet dosage form.

scholarly journals Reliable HPLC Determination of Aflatoxin M1 in Eggs

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Mostafa M. H. Khalil ◽  
Ahmed M. Gomaa ◽  
Ahmed Salem Sebaei
Keyword(s):  
Aflatoxin B1 ◽  
High Performance ◽  
Limit Of Detection ◽  
Aflatoxin M1 ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Animal Products ◽  
Liquid Chromatography Method ◽  
Different Levels

Aflatoxin M1 is the foremost metabolite of aflatoxin B1 in humans and animals, which may be present in animal products from animals fed with aflatoxin B1 contaminated feed. In this study a high performance liquid chromatography method for determination of aflatoxin M1 in eggs was described. The egg samples were diluted with warmed water and the toxin was immunoextracted followed by fluorescence detection. The average recovery of aflatoxin M1 at the three different levels 0.05, 0.1, and 0.5 μg/kg varied between 87% and 98%. The method is linear from the limit of quantification 0.05 μg/kg up to 3 μg/kg levels. This method is intended for aflatoxin M1 analyses in eggs simply with minimum toxin lose, excellent recovery, and accurate results with the limit of detection 0.01 μg/kg.

scholarly journals A Quantitative, Sensitive and Rapid Validated Analytical RP-HPLC Method for the Estimation of Dapagliflozin in Bulk and Pharmaceutical Dosage Formulations

2020 ◽  
Vol 11 (2) ◽  
pp. 2543-2548
Author(s):  
Gouru Santhosh Reddy ◽  
Animesh Bera ◽  
Madhurima Basak ◽  
Krishnaveni Nagappan ◽  
Ramalingam Peraman
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Current Method ◽  
Hplc Method ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Rp Hplc ◽  
Pharmaceutical Industries ◽  
Liquid Chromatography Method

The present study is aimed to develop a linear, precise, and accurate RP-HPLC (Reverse Phase High-Performance Liquid Chromatography) method for the determination of dapagliflozin in the formulation. The method was accomplished on a C18 column (250×4.6mm; 5µm), & Samples were eluted using acetonitrile: water (40:60%v/v) delivered at a flow rate of 1.0ml/min with a chromatographic run time of 10 min. The eluents were observed utilizing a UV detector with a wavelength set at 277nm. The method that was developed resulted in the retention of dapagliflozin at 7.029minutes. Dapagliflozin through current method has shown linearity (r2 > 0.999) over the concentration range of 1-16 µg/ml. The percentage recovery was observed to be within the limits of 98-102%, demonstrating the accuracy of the method. Limit of detection (LOD) and limit of quantification (LOQ) were qualified at 0.049µg/ml and 0.1485µg/ml, respectively. A Linear, precise, accurate, simple, and rapid RP-HPLC method has been developed and validated for the evaluation of dapagliflozin in bulk drug and tablet dosage forms (5mg &10mg) according to ICH Q2(R1) rules. Additionally, the proposed method could be of use in quality control tests of dapagliflozin in pharmaceutical industries.

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