scholarly journals Ion Chromatographic Method for the Simultaneous Determination of Anions and Cations in Firecrackers and Matches Samples as Known Potential Explosives

2019 ◽  
Vol 15 (1) ◽  
pp. 138
Author(s):  
Muhammad Amin ◽  
Lee Wah Lim

<p class="Abstract">A reference ion chromatography method based on column switching has been presented for the simultaneous determining anions (Cl<sup>−</sup>, ClO<sub>3</sub><sup>−</sup>, NO<sub>2</sub><sup>−</sup>, SO<sub>4</sub><sup>2</sup><sup>−</sup>, and NO<sub>3</sub><sup>−</sup>) and/or cations (NH<sub>4</sub><sup>+</sup>, Na<sup>+</sup>, K<sup>+</sup>, Ca<sup>2+</sup>, and Mg<sup>2+</sup>) using one pump, one type of mobile phase, and one detector. The reference method performed anion-exchange column and cation-exchange column and arranged serially via one 10-port valve. The determination of either anions or cations in one determination system could be made by switching the valve. When the use of 1.25 mM trimellitic acid as a mobile phase and the instrument was operated at a flow rate of 0.6 mL/min, five anions and five cations were determined on the anion-exchange column and the cation-exchange column, respectively. All anions target could be determined completely within 55 minutes, whereas the cations target could be determined within 35 minutes. The calculation of limit of detection using S/N=3 was 3.85 − 14.10 µM for anions and 2.95 − 10.58 µM for cations. The relative standard deviations of all ions were less than 3.82%, 3.29%, and 3.21% for retention time, peak area, and peak height, respectively. The reference method was then applied for the simultaneous determining anions and/or cations contained in firecrackers and matches samples as known potentially explosives.</p>

1971 ◽  
Vol 17 (9) ◽  
pp. 867-871 ◽  
Author(s):  
J I Routh ◽  
R E Bannow ◽  
R W Fincham ◽  
J L Stoll

Abstract L-Dopa and its major metabolites were separated from daily 24-h urines from patients with Parkinson’s disease, who were being treated with increasing doses of the drug, up to 4 g per day. An aliquot of each sample was passed through three different ion-exchange columns. Catecholamines (dopamine, epinephrine, norepinephrine, metanephrine, and normetanephrine) were retained on a cation-exchange column, eluted with boric acid, and quantitated by fluorometric analysis. Catechol acids, present in the effluent of the cation-exchange column, were retained on an anion-exchange column. An aliquot of the eluate of the anion-exchange column was used for colorimetric determination of 3,4-dihydroxyphenylacetic acid, while the effluent from this column was used for colorimetric determination of dopa. A second aliquot of the eluate from this column was passed over a column of alumina, which retained all the acidic metabolites except homovanillic acid, which was measured fluorometrically in the effluent from the alumina column. Vanilmandelic acid was determined in another aliquot of each urine sample by use of paper electrophoresis. The excretion pattern elicited suggests a major metabolic pathway for the L-dopa administered to patients with Parkinson's disease.


2017 ◽  
Vol 9 (2) ◽  
pp. 34
Author(s):  
N. Balaji ◽  
Sayeeda Sultana

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.


Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  

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.


2013 ◽  
Vol 3 (1) ◽  
pp. 208-210
Author(s):  
Nia Kristiningrum ◽  
Ellsy Novita Martyanti

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


2011 ◽  
Vol 2011 ◽  
pp. 1-5
Author(s):  
Ayushi D. ◽  
Arijit Sengupta ◽  
Sangita D. Kumar ◽  
A. G. Kumbhar ◽  
G. Venkateswaran

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.


2003 ◽  
Vol 791 (1-2) ◽  
pp. 73-83 ◽  
Author(s):  
Maria Beatriz de la Calle Guntiñas ◽  
René Wissiack ◽  
Guy Bordin ◽  
Adela Rosa Rodrı́guez

1956 ◽  
Vol 34 (7) ◽  
pp. 921-925 ◽  
Author(s):  
J. R. McCallum

For the determination of sulphate ion in samples containing 3 to 20 mgm., it was found that the standard precipitation techniques did not give sufficiently accurate results, and were time consuming. Reference to the literature showed that with certain modifications a complexometric method proposed by Schwarzenbach etal. for samples containing 20 to 50 mgm. of sulphate was most likely to give accurate results rapidly. In this method the sample is passed through a cation exchange column and washed with distilled water into a flask. This solution is boiled and precipitated with excess standard disodium ethylenediaminetetracetate in the presence of alcohol and ammonia using phthalein purple indicator. Provided that the details of procedure described in this paper are closely adhered to, accuracy is usually within two per cent. Calcium, magnesium, and barium may also be titrated directly using the phthalein purple indicator.


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