scholarly journals Robustness evaluation of the chromatographic determination of verapamil hydrochloride

Author(s):  
L. S. Logoyda

The aim of this study was the rubustness evaluation of the chromatographic determination of verapamil hydrochloride using Youden’s test.Methods: Youden’s test is a reliable method to evaluate the robustness of analytical methods, by means of an experiment design which involves seven analytical parameters combined in eight tests. In the present study, we assessed the robustness of a chromatographic method to quantify verapamil hydrochloride using Youden’s test. Hence, it was possible to determine the effect of each analytical parameter in the final analysis results. Youden’s test showed to be a simple and feasible procedure to evaluate the robustness of chromatographic methods.Results: Using the criteria of Youden’s test, the chromato­graphic method showed to be highly robust regarding the verapamil hydrochloride content, when variations in seven analytical parameters were introduced. The highest variation in the verapamil hydrochloride content was 0.26 %, when the concen­tration of triethylamine in the mobile phase was altered; a value considerably low and not significant in routine analyses.Conclusion: Youden’s test showed to be a reliable and useful tool for the robustness evaluation of the chromatographic method for verapamil hydrochloride quantitation. By means of this test, it was possible to evaluate the effect of seven analytical parameters in the final result of the analyses. Therefore, Youden’s test can be successfully applied for the ro­bustness evaluation in validation process of analytical methods by HPLC.

Author(s):  
K. Peleshok ◽  
O. Dutchak ◽  
Fatma Abdelmalek Mohamed

The robustness of an analytical procedure is a measure of its capacity to remain unaffected by small, but deliberate variations in method parameters and provides an indication of its reliability during normal usage. The aim of the study – to evaluate the rubustness of HPLC determination of valsartan in tablets using Youden’s test. Material and Methods. An efficient method to assess the robustness of analytical methodsis by Youden’s test, by means of an experiment design which involves seven analytical parameters combined in eight tests. In the recent studies, we assessed the robustness of a chromatographic method to quantify valsartan in tablets using Youden’s test. Results. The experimental design approach (design of experiment) is the method of simultaneous investigation of the influence of several factors on robustness of the method using a certain plan (matrix) of experiments. By using the Youden’s test criteria, HPLC method showed to be greatly robust concerning valsartan content, at the introduction of variation in seven analytic parameters. This was done in order to make analytical scientists more successful and businesses more profitable and productive. Conclusion. Youden’s test proved to be an efficient and helpful tool for the robustness evaluation for assay of valsartan by HPLC. Youden’s test can be applied successfully for the robustness evaluation in validation process of analytical methods.


1971 ◽  
Vol 54 (1) ◽  
pp. 175-177
Author(s):  
Judith A Armour ◽  
Jerry A Burke

Abstract Chlorinated naphthalenes are industrial chemicals with properties similar to those of polychlorinated biphenyls (PCB); they are recovered from foods by analytical methods for multiple residues of organochlorine pesticides. The chlorinated naphthalenes may interfere with the gas chromatographic determination of several organochlorine pesticides. A silicic acid column chromatographic method previously developed to separate PCB from organochlorine pesticide residues, particulary DDT and its analogs, also separates chlorinated naphthalenes from the pesticides and permits GLC determination without interference.


2009 ◽  
Vol 45 (2) ◽  
pp. 235-240 ◽  
Author(s):  
Isabela da Costa César ◽  
Gerson Antônio Pianetti

Youden's test is a reliable method to evaluate the robustness of analytical methods, by means of an experiment design which involves seven analytical parameters combined in eight tests. In the present study, we assessed the robustness of a chromatographic method to quantify lumefantrine in raw material samples, using Youden's test. Hence, it was possible to determine the effect of each analytical parameter in the final analysis results. Youden's test showed to be a simple and feasible procedure to evaluate the robustness of chromatographic methods.


1985 ◽  
Vol 68 (3) ◽  
pp. 493-494
Author(s):  
Masatoshi Yamamoto ◽  
Masaaki Ishikawa ◽  
Toshio Masui ◽  
Hiroyuki Nakazawa ◽  
Yozo Kabasawa

Abstract A simple and rapid liquid chromatographic method is described for the determination of barbaloin (aloin, 10-D-gIucopyranosyl-l,8-dihydroxy- 3-(hydroxymethyI)-9(10#)-anthracenone) in foods. Barbaloin is extracted with water from foods containing aloe and the extract is cleaned up on a disposable cartridge by using methanol-water (55 + 45) as eluant. The eluted barbaloin is separated by liquid chromatography on a YMC A-302 column with methanol-water (50 + 50) mobile phase, and detected at 293 nm. Recoveries of barbaloin added to foods at the levels of 0.05 and 0.50 mg/g were 94.4-100%. Assay results for commercial food samples indicated that the present method is applicable to a variety of foods supplemented with aloe.


1992 ◽  
Vol 75 (5) ◽  
pp. 809-811 ◽  
Author(s):  
Robert J Gargiullo

Abstract A simple, rapid liquid chromatographic method is described for quantitative determination of sucralfate in dental cream. Analyses were performed on a weak anion exchange column with 0.6M ammonium sulfate-0.005M tetrabutylammonium hydrogen sulfate as the mobile phase and refractive index detection. The method was linear over a range of 0.0 to 20.0% sucralfate in dental cream. The coefficient of variation was 3.2%. Standard recoveries were concentration dependent and ranged from 97.2 to 104.9%.


2001 ◽  
Vol 84 (2) ◽  
pp. 493-497 ◽  
Author(s):  
Richard D Thompson ◽  
John T Quaife

Abstract A liquid chromatographic method was developed that provides a simple and rapid means of determining methyl anthranilate (MA) in carbonated and noncarbonated, artificial grape-flavored, nonalcoholic beverages. The proposed procedure, which was applied to 12 different products, uses a Nova-Pak C18 column, a mobile phase containing acetonitrile–0.025M KH2PO4 (40 + 60), pH 3.00, and UV detection at 220 nm. Assay values ranged from 0.35 to 16.6 Μg MA/mL. The intralaboratory precision (relative standard deviation) for the products ranged from 0.51 to 2.23% (n = 5), and recoveries via fortification ranged from 83.6 to 102.4%. The limits of quantitation and detection were 0.00417 and 0.00125 μg/mL, respectively, and the analyte response was linear over a 100-fold concentration range (0.0001–0.01 mg/mL).


2019 ◽  
Vol 70 (6) ◽  
pp. 2015-2020
Author(s):  
Silvia Robu ◽  
Aurelia Romila ◽  
Olimpia Dumitriu Buzia ◽  
Adrian Florin Spac ◽  
Camelia Diaconu ◽  
...  

Numerous articles on Salvia officinalis L. have been published regarding the composition of their essential oil. The considerable variation found may be due to the quality of the plant material as well as to the methods used for analysis. A simple GC-MS method was developed and optimized in the QbD approach, for the determination of sage essential oils. The optimization of GC-MS analysis was performed using different mobile phase flows, injection volumes, split ratios and temperature programs. The optimized method proved to be simple and can be successfully applied for the determination of sage essential oils.


2019 ◽  
Vol 15 (6) ◽  
pp. 635-641
Author(s):  
Nadia M. Mostafa ◽  
Ghada M. Elsayed ◽  
Nagiba Y. Hassan ◽  
Dina A. El Mously

Background:The concept of green analytical chemistry prevails due to the growing environmental pollution.Objective:Our attempts are to develop simple and eco-friendly method which is non-harmful to the environment by producing minimal waste. In this context, a green liquid chromatographic method was applied for the simultaneous determination of chlorpheniramine maleate, pseudoephedrine hydrochloride and propyphenazone in their combined dosage form.Methods:Separation was carried out using X select HSS RP C18 analytical column (250 × 4.6 mm, 5μm) using methanol - 0.02 M phosphate buffer pH 3 - triethylamine (60:40: 0.1, by volume) as a mobile phase. The separated peaks were detected at 215 nm at a flow rate 1.0 mL/min.Results:Quantification was done over the concentration ranges of 1-25 µg/mL for chlorpheniramine maleate, 5-35 µg/mL for pseudoephedrine hydrochloride and 10-120 µg/mL for propyphenazone. The suggested method was validated with regard to linearity, accuracy and precision according to the International Conference on Harmonization guidelines with good results.Conclusion:It could be used as a safer alternative for routine analysis of the mentioned drugs in quality control laboratories.


1984 ◽  
Vol 49 (10) ◽  
pp. 2349-2354 ◽  
Author(s):  
František Vláčil ◽  
Karel Koňák

The selectivity coefficients of the nitrate and chloride ions and of anionic chloro complexes of Au(III), Rh(III), Pd(II), and Pt(IV) for ion exchange on Spheron DEAE in the chloride form are determined by the dynamic method. the complex anion species formed are identified and the ion exchange nature of the sorption of precious metals on this sorbent is confirmed based on the elution order of the precious metals as determined previously by the column chromatography on Spheron DEAE using hydrochloric acid as the mobile phase. The effect of the presence of perchlorate in the mobile phase during the liquid chromatography of precious metals and during the chromatographic determination of nitrate traces is explained.


1971 ◽  
Vol 54 (3) ◽  
pp. 711-712
Author(s):  
Martha Fuzesi

Abstract A gas chromatographic method is described for the quantitative determination of N-butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-tolindine and α,α,α-trifluoro-2,6-dinitro-N,N-dipropyI-p-toluidine herbicides in formulations. The sample is extracted with benzene, and equal amounts of sample and reference solution in the same concentration range are analyzed by gas chromatography, using an electron capture detector and an SE-30/Diatoport S column. The method has been applied successfully to laboratory-prepared and commercial samples.


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