scholarly journals YOUDEN'S TEST FOR CHROMATOGRAPHIC DETERMINATION OF ENALAPRIL IN PHARMACEUTICALS

2020 ◽  
Vol 5 (2) ◽  
pp. 83-87
Author(s):  
L. S. Logoyda
Keyword(s):  
Chromatographic Method ◽  
Holistic Approach ◽  
Chromatographic Determination ◽  
Hplc Method ◽  
Hplc Assay ◽  
Particle Technology ◽  
Interlaboratory Studies ◽  
Validation Procedure ◽  
First Time

Background. Robustness tests were firstly introduced for avoiding problems in interlaboratory studies and identifying the factors potentially responsible. A robustness test performing in late validation procedure involves the possibility that when the method is established not robust, it should be redeveloped and optimized. At this stage much effort has been made and money spent for optimization and validation, and therefore avoiding this would be great. Objective. The aim of the study was to consider the robustness of HPLC determination of enalapril (in tablets) by the Youden’s test. Methods. Youden’s test was chosen as an efficient method to assess the robustness among all analytical methods that is by means of an experiment design, which involved seven analytical parameters combined in eight tests. In previous studies, we evaluated the chromatographic method robustness to quantify enalapril (in tablets) by Youden’s test. Results. According to the Youden’s test criteria, HPLC method proved to be greatly robust regarding the enalapril content in introduction of variation of seven analytic parameters. The lowest variation in enalapril content was 0.91 %, when Grace Platinumр C8 EPS column (4.6 mm i.d. X 250 mm, 5 μm) was used. A holistic approach concerning simultaneous innovations in particle technology and instrument design was endeavored for the first time to meet and tackle the analytical laboratory issues. This was aimed at promoting success of analytical scientists as well as profitability and productiveness of business.  Conclusion. The Youden’s test has been proved to be an efficient and useful tool for evaluation of robustness of enalapril HPLC assay.

scholarly journals ROBUSTNESS EVALUATION OF THE CHROMATOGRAPHIC DETERMINATION OF VALSARTAN IN PHARMACEUTICALS

2020 ◽  
pp. 26-31
Author(s):  
K. Peleshok ◽  
O. Dutchak ◽  
Fatma Abdelmalek Mohamed
Keyword(s):  
Experimental Design ◽  
Efficient Method ◽  
Chromatographic Method ◽  
Analytical Procedure ◽  
Chromatographic Determination ◽  
Hplc Method ◽  
Validation Process ◽  
Helpful Tool ◽  
Test Criteria

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.

scholarly journals Development of a HPLC Method for the Quantitative Determination of Capsaicin in Collagen Sponge

2015 ◽  
Vol 2015 ◽  
pp. 1-6 ◽  
Author(s):  
Chun-Lian Guo ◽  
Hong-Ying Chen ◽  
Bi-Ling Cui ◽  
Yu-Huan Chen ◽  
Yan-Fang Zhou ◽  
...  
Keyword(s):  
Ultrasonic Wave ◽  
Extraction Method ◽  
Chromatographic Method ◽  
Pharmaceutical Products ◽  
Hplc Method ◽  
Collagen Sponge ◽  
Hplc Assay ◽  
The Mean ◽  
Perfect Recovery

Controlling the concentration of drugs in pharmaceutical products is essential to patient’s safety. In this study, a simple and sensitive HPLC method is developed to quantitatively analyze capsaicin in collagen sponge. The capsaicin from sponge was extracted for 30 min with ultrasonic wave extraction technique and methanol was used as solvent. The chromatographic method was performed by using isocratic system composed of acetonitrile-water (70 : 30) with a flow rate of 1 mL/min and the detection wavelength was at 280 nm. Capsaicin can be successfully separated with good linearity (the regression equation isA= 9.7182C+ 0.8547;R2= 1.0) and perfect recovery (99.72%). The mean capsaicin concentration in collagen sponge was 49.32 mg/g (RSD = 1.30%;n= 3). In conclusion, the ultrasonic wave extraction method is simple and the extracting efficiency is high. The HPLC assay has excellent sensitivity and specificity and is a convenient method for capsaicin detection in collagen sponge. This paper firstly discusses the quantitative analysis of capsaicin in collagen sponge.

High Pressure Liquid Chromatographic Determination of Uncombined Intermediates in FD&C Red No. 2

1977 ◽  
Vol 60 (1) ◽  
pp. 173-175
Author(s):  
Manjeet Singh
Keyword(s):  
High Pressure ◽  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Hplc Method ◽  
Disulfonic Acid ◽  
High Pressure Liquid Chromatographic ◽  
Time Required ◽  
Liquid Chromatographic ◽  
Column Chromatographic

Abstract A high pressure liquid chromatographic (HPLC) method is presented for the separation and determination of uncombined intermediates in FD&C Red No. 2 (amaranth). Samples of FD&C Red No. 2 containing 0.1—0.3% naphthionic acid, 0.1—0.4% 2-naphthol-3,6-disulfonic acid, 0.3—1.0% 2-naphthol-6,8-disulfonic acid, and 2-naphthol-3,6,8-trisulfonic acid were prepared and analyzed by HPLC. Recoveries ranged between 92 and 101%. Twenty samples of FD&C Red No. 2 were analyzed by the conventional column chromatographic method and the HPLC method. The HPLC method was superior, since it separated all the above intermediates from each other and from FD&C Red No. 2 in one quarter the time required by the conventional column chromatographic method which did not separate the individual intermediates.

Gas Chromatographic Determination of N-Butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-toluidine and α,α,α-Trifluoro-2,6-dinitro-N,N-dipropyl-p-toluidine in Formulations

1971 ◽  
Vol 54 (3) ◽  
pp. 711-712
Author(s):  
Martha Fuzesi
Keyword(s):  
Gas Chromatography ◽  
Quantitative Determination ◽  
Electron Capture ◽  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Electron Capture Detector ◽  
Reference Solution ◽  
Gas Chromatographic Method

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.

scholarly journals Robustness evaluation of the chromatographic determination of verapamil hydrochloride

2017 ◽  
Author(s):  
L. S. Logoyda
Keyword(s):  
Analytical Methods ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Final Analysis ◽  
Chromatographic Determination ◽  
Validation Process ◽  
Verapamil Hydrochloride ◽  
A Value ◽  
Analytical Parameter

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.

Gas Chromatographic Determination of Thiouracils in Feeds

1965 ◽  
Vol 48 (5) ◽  
pp. 908-911
Author(s):  
Arnaldo Fravolini ◽  
Alfredo Begliomini
Keyword(s):  
Chromatographic Separation ◽  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Methyl Silicone ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatographic method has been used to determine thiouracils added to feeds. The chromatographic separation is carried out on alkylated compounds. A column of SE-30 polymer methyl silicone was used. Recoveries averaged between 92 and 103%. The procedure is simple and brief.

scholarly journals Gas Chromatographic Determination of Chlorothalonil in Leaves and Roots of Scrophularia and in Soil

1996 ◽  
Vol 79 (2) ◽  
pp. 587-588 ◽  
Author(s):  
Lan Zhao ◽  
De-Fang Fan
Keyword(s):  
Electron Capture ◽  
Chromatographic Method ◽  
Detection Limits ◽  
Chromatographic Determination ◽  
Soil Samples ◽  
Florisil Column ◽  
Glass Column ◽  
Leaves And Roots ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method is described for determination of chlorothalonil residues in leaves and roots of Scrophularia and in soil. Samples were extracted with acetone and cleaned up on a Florisil column. Chlorothalonil residues are chromatographed directly on a glass column of 1.5% OV-17 and 2% QF-1 coated on 80-100 mesh Chromosorb W (HP) support and measured with a 63Ni electron capture detector. Detection limits are 0.001 ppm for leaf, 0.005 ppm for root, and 0.001 ppm for soil.

Capillary Column Gas Chromatographic Determination of Trace Residues of the Herbicide Chlorsulfuron in Agricultural Runoff Water

1987 ◽  
Vol 70 (4) ◽  
pp. 745-748
Author(s):  
Uaz Ahmad
Keyword(s):  
Gas Chromatography ◽  
Chromatographic Method ◽  
Capillary Column ◽  
Methylene Chloride ◽  
Chromatographic Determination ◽  
Agricultural Runoff ◽  
Runoff Water ◽  
Florisil Column ◽  
Gas Chromatographic Method

Abstract A capillary column gas chromatographic method is described for determining parts-per-trillion (ppt) levels of chlorsulfuron in agricultural runoff water. The water sample is acidified with acetic acid and extracted with methylene chloride. The chlorsulfuron in the extract is derivatized to its monomethyl derivative. After Florisil column cleanup, the methylated chlorsulfuron is determined by electron-capture gas chromatography. Recovery of chlorsulfuron from fortified water samples is greater than 80%. Detection limit of the method is 25 ng chlorsulfuron/L water (25 ppt). There are 2 reaction sites on the chlorsulfuron molecule, both of which are susceptible to methylation leading to monomethyl chlorsulfuron and dimethyl chlorsulfuron. A procedure is described to methylate selectively the sulfonamide nitrogen of chlorsulfuron.

Gas Chromatographic Determination of Histapyrrodine Hydrochloride in Pharmaceutical Preparations

1986 ◽  
Vol 69 (4) ◽  
pp. 612-613
Author(s):  
Ramesh T Sane ◽  
Vipul J Doshi ◽  
Sanjay K Joshi ◽  
Vijay K Shastri ◽  
Dhananjay S Sapre ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
Chromatographic Determination ◽  
Chlorpheniramine Maleate ◽  
Accuracy And Precision ◽  
Label Claim ◽  
Gas Chromatographic Method

Abstract A simple gas chromatographic method is described for the determination of histapyrrodine HC1 in marketed formulations. Chlorpheniramine maleate is used as the internal standard. The amount of histapyrrodine HC1 found by the proposed method averaged 19.91 mg/tablet, compared with the label claim of 20 mg/tablet. The method was statistically evaluated for accuracy and precision.

scholarly journals Gas Chromatographic Determination of Butylated Hydroxyanisole (BHA) and Butylated Hydroxytoluene (BHT) in Products Containing Capsaicinoids

1996 ◽  
Vol 79 (6) ◽  
pp. 1459-1462
Author(s):  
Bernard DeWitt ◽  
Gunnar Finne
Keyword(s):  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Butylated Hydroxytoluene ◽  
Butylated Hydroxyanisole ◽  
Liquid Chromatographic Method ◽  
Gas Chromatographic Method ◽  
Liquid Chromatographic

Abstract Because of interference by coeluting capsaicinoids, the commonly used liquid chromatographic method for determining butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) in pepperoni and spice blends is not reliable. A gas chromatographic method is described that cleanly separates these antioxidants from interfering substances. Average recoveries of BHA and BHT from oleoresin spiked at 5 concentrations were 97.6 and 104.3%, respectively. From pepperoni spiked at 4 levels, average recoveries were 79.1 and 87.9%, respectively. The repeatability of the method when applied to 5 replicates of pepperoni toppings was 36.4 ± 1.1 ppm for BHA and 32.2 ± 0.8 ppm for BHT.

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