scholarly journals Derivatization Ion Chromatography for the Determination of Monoethanolamine in Presence of Hydrazine in PHWR Steam-Water Circuits

2011 ◽  
Vol 2011 ◽  
pp. 1-5
Author(s):  
Ayushi D. ◽  
Arijit Sengupta ◽  
Sangita D. Kumar ◽  
A. G. Kumbhar ◽  
G. Venkateswaran
Keyword(s):  
Ion Chromatography ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Accurate Method ◽  
Feed Water ◽  
Relative Standard ◽  
Conductometric Detection ◽  
Mode A ◽  
Eluent Acetone

A simple, rapid and accurate method for the determination of monoethanolamine (MEA) in PHWR steam-water circuits has been developed. MEA is added in the feed water to provide protection against corrosion while hydrazine is added to scavenge dissolved oxygen. The quantitative determination of MEA in presence of hydrazine was accomplished using derivatization ion chromatography with conductometric detection in nonsuppressed mode. A Metrosep cation 1-2 analytical column and a Metrosep cartridge were used for cation separation. A mixture of 4 mM tartaric acid, 20% acetone and 0.05 mM HNO3was used as eluent. Acetone in the mobile phase leads to the formation of different derivatives with MEA and hydrazine. The interferences due Na+and NH4 +were eliminated by adopting a simple pretreatment procedure employing OnGuard-H cartridge. The limit of detection limit of MEA was 0.1 μg mL−1and the relative standard deviation was 2% for the overall method. The recovery of MEA added was in the range 95%–102%. The method was applied to the determination of MEA in steam generator water samples.

scholarly journals SENSITIVE DETERMINATION OF RELATED SUBSTANCES IN PIOGLITAZONE HYDROCHLORIDE BY HPLC

2017 ◽  
Vol 9 (2) ◽  
pp. 34
Author(s):  
N. Balaji ◽  
Sayeeda Sultana
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Internal Diameter ◽  
Related Substances ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.

scholarly journals Development and validation of reversed phase high performance liquid chromatography (RP-HPLC) for quantification of captopril in rabbit plasma

2020 ◽  
Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Rabbit Plasma ◽  
Rp Hplc ◽  
Relative Standard

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.

scholarly journals Validated TLC-densitometry method for determination of cetirizine dihydrochloride in tablet dosage form

2013 ◽  
Vol 3 (1) ◽  
pp. 208-210
Author(s):  
Nia Kristiningrum ◽  
Ellsy Novita Martyanti
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Pharmaceutical Journal ◽  
Limit Of Quantification ◽  
Quality Control Testing ◽  
Relative Standard ◽  
Tablet Formulations ◽  
Tablet Dosage ◽  
Chloroform Methanol

A rapid, reproducible and accurate TLC method was developed for the determination of Cetirizine Dihydrochloride in tablet. The analytes were dissolved with ethanol 70% and chromatographed on silica Gel GF 254 TLC plate using chloroform : methanol : ethyl acetate in the ratio of 2 : 7 : 3 (v/v) as mobile phase. Quantitative analysis was done through densitometric measurement at wavelength 234 nm. Method was found linear over the concentration range of 400 – 1600 ng/spot with the correlation coefficient of 0.996. 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 75.54 and 226.64 ng/spot. The relative standard deviation of this method was 0.86% whereas the means of the recovery data was 100.54 ± 0.11%. The proposed method has been applied to the determination of Cetirizine Dihydrochloride in commercial tablet formulations and the result were 96.97 ± 0.86 % for brand A and 100.57 ± 1.17 % for brand B. The developed method was successfully used for the assay of Cetirizine Dihydrochloride. This 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.v3i1.17294 International Current Pharmaceutical Journal, December 2013, 3(1): 208-210

scholarly journals Determination of cyanide in bamboo shoots by microdiffusion combined with ion chromatography–pulsed amperometric detection

2018 ◽  
Vol 5 (4) ◽  
pp. 172128 ◽  
Author(s):  
Ming Ding ◽  
Kailiang Wang
Keyword(s):  
Ion Chromatography ◽  
Limit Of Detection ◽  
Correlation Coefficients ◽  
Amperometric Detection ◽  
High Sensitivity ◽  
Practical Method ◽  
Pulsed Amperometric Detection ◽  
Bamboo Shoots ◽  
Relative Standard

A practical method for the determination of cyanide in bamboo shoots has been developed using microdiffusion preparation integrated with ion chromatography–pulsed amperometric detection (IC-PAD). Cyanide was released from bamboo shoots after Conway cell microdiffusion, and then analysed by IC-PAD. In comparison with the previously reported methods, derivatization and ion-pairing agent addition were not required in this proposed microdiffusion combined with IC-PAD method. The microdiffusion parameters were optimized including hydrolysis systems, temperature, time, and so on. Under the optimum conditions, the linear range of the calibration curve for cyanide was 0.2–200.0 µg kg −1 with satisfactory correlation coefficients of 0.9996 and the limit of detection was 0.2 µg kg −1 ( S/N  = 3). The spiked recovery range was from 92.8 to 98.6%. The intra-day and inter-day relative standard deviations of cyanide were 2.7–14.9% and 3.0–18.3%, respectively. This method was proved to be convenient in operation with high sensitivity, precision and accuracy, and was successfully applied in the determination of cyanide in bamboo shoot samples.

scholarly journals Determinación de F-, CL-, NO3- y SO42- en muestras de agua, por cromatografía iónica y métodos tradicionales

2017 ◽  
Vol 2 (2) ◽  
pp. 39
Author(s):  
Danis Pirela ◽  
Gleidy Vivas ◽  
Ligbel Sánchez ◽  
Hendrik Avila
Keyword(s):  
Ion Chromatography ◽  
Limit Of Detection ◽  
Comparison Of Methods ◽  
Chromatography Method ◽  
Sulfate Ions ◽  
Palabras Clave ◽  
Relative Standard ◽  
Scientific Technical ◽  
Chloride Sulfate

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

scholarly journals HPLC determination of Escitalopram in tablet dosage forms

Pharmacia ◽  
2022 ◽  
Vol 69 (1) ◽  
pp. 21-24
Author(s):  
Stefan Balkanski
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Phase Liquid ◽  
Tablet Dosage ◽  
Liquid Chromatographic

Purpose: A simple, specific, precise, and accurate reversed phase liquid chromatographic (RP-LC) method has been developed for the determination of Escitalopram in tablet dosage form. Methods: The chromatographic separation was achieved on a LiChrosorb C18, 250 mm x 4.6 mm, 5 μm column at a detector wavelength of 270 nm and a flow rate of 1.0 ml/min. The mobile phase was composed of methanol, acetonitrile (70:30 v/v). The retention time of Escitalopram was 5.49 min. The method was validated for the parameters like specificity, linearity, precision, accuracy, limit of quantitation and limit of detection. Results: The method was found to be specific as no other peaks of impurities and excipients were observed. The square of correlation coefficient (R2) was 0.9999 while relative standard deviations were found to be <2.0%. Conclusion: The proposed RP-LC method can be applied for the routine analysis of commercially available formulations of Escitalopram.

Ion chromatography as highly suitable method for rapid and accurate determination of antibiotic fosfomycin in pharmaceutical wastewater

2014 ◽  
Vol 69 (10) ◽  
pp. 2014-2022 ◽  
Author(s):  
Ping Zeng ◽  
Xiaolin Xie ◽  
Yonghui Song ◽  
Ruixia Liu ◽  
Chaowei Zhu ◽  
...  
Keyword(s):  
Ion Chromatography ◽  
Industrial Wastewater ◽  
High Performance ◽  
Limit Of Detection ◽  
Batch Reactor ◽  
Accurate Determination ◽  
Pharmaceutical Wastewater ◽  
Relative Standard ◽  
High Detection Limit

A rapid and accurate ion chromatography (IC) method (limit of detection as low as 0.06 mg L−1) for fosfomycin concentration determination in pharmaceutical industrial wastewater was developed. This method was compared with the performance of high performance liquid chromatography determination (with a high detection limit of 96.0 mg L−1) and ultraviolet spectrometry after reacting with alizarin (difficult to perform in colored solutions). The accuracy of the IC method was established in the linear range of 1.0–15.0 mg L−1 and a linear correlation was found with a correlation coefficient of 0.9998. The recoveries of fosfomycin from industrial pharmaceutical wastewater at spiking concentrations of 2.0, 5.0 and 8.0 mg L−1 ranged from 81.91 to 94.74%, with a relative standard deviation (RSD) from 1 to 4%. The recoveries of effluent from a sequencing batch reactor treated fosfomycin with activated sludge at spiking concentrations of 5.0, 8.0, 10.0 mg L−1 ranging from 98.25 to 99.91%, with a RSD from 1 to 2%. The developed IC procedure provided a rapid, reliable and sensitive method for the determination of fosfomycin concentration in industrial pharmaceutical wastewater and samples containing complex components.

scholarly journals DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OF ESCITALOPRAM OXALATE AND FLUPENTIXOL DIHYDROCHLORIDE IN COMBINED DOSAGE FORM AND PLASMA

2021 ◽  
pp. 61-66
Author(s):  
MALATHI SELLAPPAN ◽  
DARTHI DEVAKUMAR
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Photodiode Array ◽  
Development And Validation ◽  
Potassium Dihydrogen Orthophosphate

Objective: The objective of the study was to develop a simple and rapid chromatographic method for quantification of escitalopram oxalate and flupentixol dihydrochloride in combined dosage form and plasma. Methods: The separation was achieved with a sun fire C8 [150×4.6 mm] 3.5 µm column with an isocratic mobile phase containing a mixture of potassium dihydrogen orthophosphate buffer: methanol: acetonitrile [30:60:10 v/v/v] pH adjusted to 11. The flow rate of the mobile phase was 1.5 ml/min with a Photodiode array [PDA] detection at 230 nm. Results: The HPLC method was developed and validated with respective linearity, accuracy, and precision, detection of limit, robustness, and specificity. The precision of the results stated as the relative standard deviation was below 2 %. The calibration curve was linear over a concentration range from 10-50 µg/ml for escitalopram oxalate and 1-5 µg/ml for flupentixol dihydrochloride with a correlation co-efficient 0.994 and 0.977 respectively. The accuracy of the method was demonstrated at levels in the range of 100 % and 120 % of the specification limit. The recovery of escitalopram oxalate and flupentixol dihydrochloride was found to be in the range of 90 % to 88 %, respectively. The lowest detection limits were found to be 2 µg/ml for escitalopram oxalate and 0.1 µg/ml for flupentixol dihydrochloride. The lowest quantification limits were found to be 5 µg/ml of escitalopram oxalate and 0.5 µg/ml of flupentixol dihydrochloride. Conclusion: The developed method was validated for linearity, accuracy, precision, the limit of detection and quantification, specificity. The method was applied successfully for the determination of escitalopram oxalate and flupentixol dihydrochloride in the combined dosage form and plasma.

scholarly journals Determination of Deoxynivalenol in Whole Wheat Flour and Whear Bran

2002 ◽  
Vol 85 (6) ◽  
pp. 1355-1359 ◽  
Author(s):  
Heidi S Rupp
Keyword(s):  
Wheat Flour ◽  
Wheat Bran ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Test Sample ◽  
Whole Wheat Flour ◽  
Whole Wheat ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method was developed for determining deoxynivalenol (DON) in whole wheat flour and wheat bran. A 15 g test sample was extracted with acetonitrile–water (84 + 16, v/v) and applied to a Romer MycoSep cleanup column. The eluate was dried and then reconstituted in a 0.1M phosphate buffer, pH 7.0, and applied to a Vicam DONtest-LC cleanup column. The methanol eluate was chromatographed with a methanol–water (17 + 83, v/v) mobile phase on a C18 column with UV detection at 220 nm. Five replicates at each of 5 fortification levels (0.25, 0.50, 1.0, 2.0, and 4.0 ppm), plus 5 controls, were determined for both whole wheat flour and wheat bran. For flour, the average recoveries were 72.2–91.5% with relative standard deviations (RSDs) of 4.9–18.4%. The intra-assay flour recovery was 82.4% with 9.8% RSD. A 5 replicate sample of naturally incurred wheat had an average of 1.1 ppm DON with 6.7% RSD. For bran, average recoveries of fortified samples were 69.5–99.7% with RSDs of 1.7–18.8%. The intra-assay bran recovery was 81.5% with 8.9% RSD. The limit of detection (about 3× noise) for the method is 0.05 ppm; the correlation coefficient (linearity) was >0.9995. The DON peak was clearly identified and easily integrated in the chromatograms.

scholarly journals Determination of Diazepam in Cream Biscuits by Liquid Chromatography

2004 ◽  
Vol 87 (3) ◽  
pp. 569-572 ◽  
Author(s):  
Priyankar Ghosh ◽  
Mudiam Mohanakrishna Reddy ◽  
Beedu Sashidhar Rao ◽  
Rajendra Kumar Sarin
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Internal Standard ◽  
Reversed Phase ◽  
Calibration Plot ◽  
Relative Standard ◽  
Limit Of Quantitation

Abstract An analytical procedure was developed for the detection and quantitation of diazepam in cream biscuits, which were used to commit crime. The method involves the extraction of diazepam with ethanol at room temperature, and the extract is filtered, evaporated to dryness, and redissolved in the mobile phase, methanol–acetonitrile–tetrahydrofuran–water (15 + 55 + 4 + 26, v/v). The separation is achieved on a C18 reversed-phase column with the mobile phase and diode array detection (λmax) at 230 nm. Medazepam is used as the internal standard is for quantification. The calibration plot for the determination of diazepam is based on linear regression analysis (y = 0.6687x + 0.0372; r2 = 0.995). The limit of detection for diazepam in the biscuit samples was estimated as 600 ng/mL. The limit of quantitation for diazepam was estimated as 1.75 μg/mL. The diazepam detected per piece of biscuit was found to be in the range of 0.27–0.45 mg. Pure diazepam was added to biscuit samples at 3 levels (100 and 500 μg/g, and 1 mg/g), and the recoveries were found to be 95%. The mean retention time of diazepam was 2.7 min and that of medazepam (IS) was 4 min. The relative standard deviations of the diazepam level in the biscuit samples were estimated to be 0.4% for retention time and 1.02% for peak area in intraday analysis, whereas the corresponding values were and 0.61 and 2.34% in interday analysis. The method is rapid and reliable for qualitative and quantitative analysis of cream biscuits laced with diazepam, and it can be used by law enforcement laboratories for routine analysis.

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