scholarly journals A Validated Ion Chromatography method for determination of Ammonium content in Omeprazole tablets

2014 ◽  
Vol 2 (03) ◽  
pp. 90-95
Author(s):  
Swetha C. Parshaa ◽  
Y. Ravindra Kumara ◽  
M. Ravi Chanderb

A simple, feasible, definite and strong Ion chromatography method was developed for the quantitative determination of ammonium content in Omeprazole tablets. The method was developed using Ion pac CS17 Column, 250 X 4.6mm X 5.0 m column with mobile phase containing 1.5mM Methane sulfonic acid in water. The eluted compounds were monitored using conductivity detector. The unknown peak and ammonium peak were well separated with resolution more than 2.0. The developed method was validated as per Internatonal Conference on Harmonisation of technical Requirements for registration of pharmaceuticals for human use guidelines with respect to linearity (The high correlation coefficient >0.99), limit of detection, limit of quantification, exactness, precision and robustness. The Limit of detection, Limit of quantification values of Ammonium were 8ppm and 30ppm respectively.

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>


2013 ◽  
Vol 57 (1) ◽  
pp. 25-32 ◽  
Author(s):  
Anna Gajda ◽  
Andrzej Posyniak ◽  
Andrzej Bober ◽  
Tomasz Błądek ◽  
Jan Żmudzki

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.


2016 ◽  
Vol 680 ◽  
pp. 52-55
Author(s):  
Hong Yan Guan ◽  
Jian Jun Ding ◽  
Zhong Bao Guo ◽  
Ming Yu Wang ◽  
Yi Fei Mei

The determination of chloride ions in concrete materials accurately is far and away crucial, since chloride ions can cause corrosion of steel and concrete cover off. The conventional potential method and silver nitrate titration method usually show features of simple operation and short duration, nevertheless, they are not suitable for accurate analysis for concrete attributing to their low accuracy and detection limit. In this paper, an ion chromatography method was presented to determine chlorine in concrete materials. Concrete samples were pre-processed and then extracted with distilled water. The extraction solutions were purified on a 0.22 μm filter membrane, an On Guard SPE-RP column and a SPE-H column sequentially for eliminating undissolved substance, organisms and metal ions before ion chromatographic analysis. The chromatographic separation was performed on a Dionex ICS-1000 Chromatographic using 25.0 mmol/L KOH solutions as mobile phase at 1.0 mL/min. Results show that the detection limit of the method was 0.004 mg/L. The linear relationship of the external Cl- standard solutions was 0.9994, and the sample analytical RSD was 0.44%.


2018 ◽  
Vol 2018 ◽  
pp. 1-5 ◽  
Author(s):  
Ahmed Salem Sebaei ◽  
Ahmed M. Gomaa ◽  
A. A. El-Zwahry ◽  
E. A. Emara

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.


Author(s):  
Danis Pirela ◽  
Gleidy Vivas ◽  
Ligbel Sánchez ◽  
Hendrik Avila

RESUMEN El análisis químico debe generar resultados correctos y confiables, siendo importante la validación del método para la realización de servicios científicos técnicos, con calidad de los resultados. Se determinó la concentración de los F-, Cl-, NO3- y SO42- por métodos tradicionales y cromatografía iónica. Se evaluó la precisión en término de repetibilidad y la exactitud en porcentaje de recuperación utilizando patrones certificados. Se obtuvieron desviaciones estándar relativas en un intervalo de 0,70 a 4% y porcentajes de recuperación entre 98 y 99% para el análisis por cromatografía iónica. El límite de detección para el método de cromatografía iónica se encontró entre 0,005 y 0,1391 mg/L y mostró una linealidad de 0,999. Los resultados demuestran que el método de cromatografía iónica es más sensible y rápido al ser comparado con los métodos tradicionales, con comportamientos similares para la determinación de los iones de fluoruro y sulfato, pero diferentes en la determinación de los iones de cloruro y nitrato. Palabras clave: Cromatografía iónica, fluoruro, cloruro, sulfato, nitrato, comparación de métodos. ABSTRACT Chemical analysis must generate correct and reliable results, method validation for scientific-technical services with quality results, to be important. Comparing the results obtained by traditional methods and ion chromatography in the determination of F-, Cl-, NO3- and SO42-- was conducted. Was evaluated in terms of repeatability precision and for accuracy tests of recovery using certified patterns were carried out. Relative standard deviations in a range from 0.70 to 4% and recovery rates between 98 and 99% for analysis by ion chromatography were. The limit of detection for ion chromatography method was found between 0.005 and 0.1391 mg/L and showed a linearity of 0.999. The results show that the ion chromatography method is more sensitive and faster when compared with the methods traditional, with similar behaviors for the determination of fluoride and sulfate ions, but different in the determination of the chloride and nitrate ions. Key words: Ion chromatography, fluoride, chloride, sulfate, nitrate, comparison of methods


INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (09) ◽  
pp. 68-73
Author(s):  
K Vijaya Sri ◽  
M. Shiva Kumar ◽  
M. A. Madhuri ◽  
Suresha K. ◽  

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.


2015 ◽  
Vol 7 (23) ◽  
pp. 9825-9834 ◽  
Author(s):  
Slobodan V. Jovanovic ◽  
Thomas Zakharov ◽  
Hemendra Mulye ◽  
Duck Kim ◽  
Kelly-Anne Fagan

In this study, we developed and validated a sensitive method for the determination of hydrazine in water samples using ion chromatography coupled with an amperometric detector (limit of detection (LOD) = 0.02 μg L−1 and limit of quantification (LOQ) = 0.1 μg L−1).


2020 ◽  
Vol 8 (2) ◽  
pp. 1-7
Author(s):  
Ihsan M. Shaheed ◽  
Saadiyah A. Dhahir

The quinolizindine alkaloid compound, oxymatrine pesticide, was analysis in the river water samples collected from different agriculture areas in the Iraqi city of Kerbala and also in its formulation using developed reverse-phase high-performance liquid chromatography method. Acetonitrile:methanol (60:40 v/v) was chosen as mobile phase at pH (7.0), flow rate 0.5 mL/min, and 20 µL as volume injection. Modified ecological-friendly method, dispersive liquid-liquid microextraction, was used for the extraction of oxymatrine from water samples. Linearity study was constructed from 0.1 to 70 μg/mL at λmax 205 nm. The limit of detection and limit of quantification were 0.025 and 0.082 μg/mL, respectively, and the relative standard deviation (RSD) % was 0.518%. Three spiked levels of concentration (20.0, 40.0, and 70.0 μg/mL) were used for the validation method. The percentage recovery for the three spiked samples was ranged between 98.743 and 99.432 and the RSD% was between 0.051 and 0.202%, the formulation studies of oxymatrine between 99.487 and 99.798, and the RSD% was ranged from 0.045 to 0.057%. The developed method can be used accurately and selectively for the determination of oxymatrine in environmental samples and in the formulation.


Separations ◽  
2021 ◽  
Vol 8 (11) ◽  
pp. 212
Author(s):  
Bin Jiang ◽  
Shaojing Zhong ◽  
Hongliang Yu ◽  
Peifeng Chen ◽  
Baoyun Li ◽  
...  

Thiocyanate could effectively inhibit bacteria in milk and extend the shelf life of milk. However, excessive addition will lead to health risks. Therefore, the determination of thiocyanate in raw milk has received a lot of attention, but the determination could be interfered with by other components in raw milk and the pre-treatment of raw milk is complex. In this study, a new pretreatment method combined with ion chromatography (IC) for rapid and sensitive determination of thiocyanate is proposed. An acetonitrile/(NH4)2SO4 aqueous two-phase system (ATPS) was developed for the separation and enrichment of thiocyanate in raw milk. Response surface methodology was performed to optimize the extraction conditions and an efficient pretreatment were obtained using ATPS composed of 42% acetonitrile (w/w) and 16% (NH4)2SO4 (w/w), with the pH 4.7, and the recovery of thiocyanate reached 107.24 ± 0.5%, and the enrichment ratio was 10.74 ± 0.03. IC was used to establish a thiocyanate enrichment method. The linear range was from 0.05 to 15 mg/L and R2 = 0.998, the limit of detection (LOD) was 0.2 μg/L, the limit of quantification (LQD) was 0.6 μg/L. Hence, it is feasible to combine ATPS with IC for the enrichment and determination of thiocyanate in raw milk.


2020 ◽  
Vol 17 (34) ◽  
pp. 1046-1054
Author(s):  
Ihsan Mahdi SHAHEED ◽  
Saadiyah Ahmed DHAHIR

The triazole, tebuconazole pesticide, was determined in its formulation and also in the river water samples collected from different agriculture areas in the Iraqui city of Kerbala using developed high-performance liquid chromatography method(HPLC) with UV-visible detection, The mobile composition phase was a mixture of acetonitrile:methanol (50:50 v/v) and the column was C18 (250 cm x 4.6 mm,5μm). Also modified dispersive liquidliquid microextraction (DLLME), which is regarded as an ecological -friendly method, was used for the extraction of tebuconazole from water samples using acetonitrile and chloroform as solvents extraction and dispersive agent, respectively. Linearity to maintain the calibration curve was achieved from (0.1-70) μg.mL-1 with a limit of detection(0.053) μg.mL-1 and limit of quantification (0.174) μg.mL-1. Three spiked levels of concentration (1.0, 5.0, and 10) μg.mL-1 were used for the validation of the method. The relative standard deviation (RSD%) was (0.294- 0.813)%, and the percentage recovery was (100.001-100.005). The formulation studies for two different concentrations (10 and 40) μg.mL-1, which prepared from tebuconazole formulation (Raxil ODS2 2%), gave acceptable percentage recovery between (98.956-99.833). The developed method can be used accurately for the determination of tebuconazole in water samples and in the formulation of tebuconazole effectively.


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