Optimized Chromatographic Determination of Naphazoline and Chlorpheniramine in Eye/Nose Drops Using Cation-exchange Column

2021 ◽  
Author(s):  
Imad Osman Abu Reid
Keyword(s):  
Cation Exchange ◽  
Chromatographic Determination ◽  
Naphthalene Acetic Acid ◽  
Intermediate Precision ◽  
Exchange Column ◽  
System Suitability ◽  
Liquid Chromatographic Method ◽  
Cation Exchange Column ◽  
Liquid Chromatographic

Abstract A simple and efficient liquid chromatographic method has been developed and validated for the simultaneous determination of naphazoline and chlorpheniramine in eye/nose drops, in presence of naphazoline degradation product and naphthalene acetic acid (NAPD). The separation was achieved within 6.0 min, employing a mixture of 53.5% v/v water-acetonitrile containing 78.70 mM/L sodium dihydrogen orthophosphate adjusted to pH 5.30 as isocratic mobile phase, pumped at 1.0 mL/min through a strong cation-exchange column (10 μm particle size), the analytes were monitored at 230 nm. Statistical experimental designs and graphic representations (response surface methodology) were used for optimizing the chromatographic separation. The linearity plots were linear over concentration range up to 125% of the analytes nominal concentrations (100%) with regression coefficients (r) > 0.99, method’s accuracy (RSD < 2.0%), repeatability and intermediate precision (RSD < 2.0%) were verified. System suitability parameters were also within the acceptable range. The validated method was successfully employed for the routine analysis of eye/nose drops.

Liquid Chromatographic Determination of Morphine Sulfate and Some Contaminants in Injections and Bulk Drug Material: Collaborative Study

1988 ◽  
Vol 71 (5) ◽  
pp. 1046-1048
Author(s):  
Ada C Bello ◽  
Rita K Jhangiani
Keyword(s):  
Collaborative Study ◽  
Chromatographic Determination ◽  
Morphine Sulfate ◽  
System Suitability ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Bulk Drug ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for the assay of morphine sulfate and some preservatives and impurities in the bulk drug and in injections has been developed and collaboratively studied in 8 laboratories. Each collaborator analyzed 5 samples: 1 bulk drug, 3 different concentrations of injectable dosages, and 1 prepared mixture containing, in addition to morphine sulfate, phenol, 2-mercaptobenzothiazole, and pseudomorphine. The proposed method quantitates morphine sulfate and resolves the other components for identification using a Clg reverse-phase column with a mobile solvent containing 240 mL methanol, 720 mL 0.005M 1-heptanesulfonic acid Na salt, and 10 mL acetic acid. Samples are prepared by direct dilution with mobile solvent minus 1-heptanesulfonic acid. All collaborators met system suitability requirements and performed the analysis without difficulty. No outliers were found when data were analyzed by the Dixon, Grubbs, double Grubbs, and Cochran tests. Relative standard deviations between laboratories (RSDR) for duplicate determinations of morphine sulfate ranged from 1.4 to 2.1%. Mean morphine sulfate recoveries for the bulk drug and the prepared mixture were 100.8 and 100.4%, respectively. The method has been approved interim official first action.

Liquid Chromatographic Determination of Thiamine in Infant Formula Products by Using Ultraviolet Detection

1985 ◽  
Vol 68 (6) ◽  
pp. 1087-1092
Author(s):  
Benjamin K Ayi ◽  
David A Yuhas ◽  
Kathryn S Moffett ◽  
Deidre M Joyce ◽  
Nicholas J Deangelis
Keyword(s):  
Infant Formula ◽  
Chromatographic Determination ◽  
Phosphate Esters ◽  
Exchange Column ◽  
Relative Standard ◽  
Cation Exchange Column ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Different Levels

Abstract A liquid chromatographic (LC) method has been developed for determination of thiamine in infant formula products. The method involves the following steps: (a) dissolution of the formula with water, (b) pH adjustment to induce protein precipitation, (c) filtration, (d) concentration of thiamine by using a cation exchange column and extraction system, (e) cleanup of adsorbed thiamine and other contaminants on the ion exchange column by washing with water and then methanol, (f) elution of thiamine with a mixture of methanol-2M potassium chloride buffer, (g) analysis for thiamine by liquid chromatography. Thiamine is separated from its phosphate esters, the mono-, di-, and triphosphates, as well as its antagonists oxythiamine and pyrithiamine on a 6 p-m particle size column and a mobile phase of 40mM triethylammonium phosphate buffer-methanol (pH 7.7) (90 + 10). The method is reproducible, with relative standard deviations ranging from ± 0.76 to ± 1.2%, depending on the infant formula product tested. Recovery of thiamine from various infant formula products is greater than 99%. Analysis for thiamine of several commercially available infant formulas at different levels of fortification gave results that ranged from 122 to 216% of the declared levels. These results agree well with those obtained using the AOAC fluorometric method.

High Pressure Liquid Chromatographic Determination of Saccharides in Corn Sirups: Collaborative Study

1979 ◽  
Vol 62 (3) ◽  
pp. 527-532
Author(s):  
C Earl Engel ◽  
Philip M Olinger
Keyword(s):  
Cation Exchange ◽  
Collaborative Study ◽  
Strong Acid ◽  
Chromatographic Determination ◽  
Ion Exchange Resin ◽  
Exchange Column ◽  
Coefficients Of Variation ◽  
Cation Exchange Column ◽  
Carbohydrate Components ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for quantitative analysis of saccharides in corn sirup was investigated. Fructose, glucose, and related saccharides are separated on an Aminex 50W-X4, calcium form, cation exchange column or, alternatively, on an Aminex Q15-S, calcium form, cation exchange column. Water is the solvent. All carbohydrate components in the sirup elute from the column, permitting normalized computation vs. synthetically prepared standards. The corn sirup samples are diluted to an approximate dry substance and injected directly into the chromatograph. When required, interfering ionic material is removed with the aid of a mixed strong acid-weak base ion exchange resin. The reproducibility and repeatability coefficients of variation for fructose (on samples ranging from 15 to 90% fructose) are 0.9 and 0.3%, respectively. The reproducibility and repeatability coefficients of variation for glucose (on samples ranging from 8 to 50% glucose) are 1.4 and 0.5%, respectively. The method has been adopted as official first action.

Liquid Chromatographic Fluorescence Method for the Determination of Thiabendazole Residues in Green Bananas and Banana Pulp

1994 ◽  
Vol 77 (3) ◽  
pp. 710-713 ◽  
Author(s):  
Rene V Arenas ◽  
Nelson A Johnson
Keyword(s):  
Column Liquid Chromatography ◽  
Cation Exchange ◽  
Chromatographic Method ◽  
Solid Phase ◽  
Extraction Column ◽  
Phase Extraction ◽  
Liquid Chromatographic Method ◽  
Cation Exchange Column ◽  
Liquid Chromatographic

Abstract A novel liquid chromatographic method was developed for the determination of thiabendazole (TBZ) residues in whole green bananas and ripe banana pulp. TBZ is extracted from the banana matrix with ethyl acetate, followed by cleanup of extract on a cation-exchange, solid-phase extraction column. The extract is analyzed for TBZ residues by column liquid chromatography using a cation-exchange column with fluorescence detection. Recoveries of TBZ from whole green bananas fortified with TBZ at 0.05-10 ppm and from ripe banana pulp fortified with TBZ at 0.01-2 ppm averaged 93 and 95%, respectively. The following method for monitoring TBZ residues in whole green bananas and ripe banana pulp is simple, rapid, and sensitive.

Liquid Chromatographic Determination of Amiodarone Hydrochloride and Related Compounds in Raw Materials and Tablets

1994 ◽  
Vol 77 (6) ◽  
pp. 1447-1453 ◽  
Author(s):  
Pauline M Lacrok ◽  
Norman M Curran ◽  
Wing-Wah Sy ◽  
Dennis K J Goreck ◽  
Pierre Thibault ◽  
...  
Keyword(s):  
Raw Materials ◽  
Chromatographic Determination ◽  
Raw Material ◽  
Liquid Chromatographic Method ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Amiodarone Hydrochloride ◽  
Related Compounds

Abstract A liquid chromatographic method for the determination of amiodarone hydrochloride and 10 related compounds in drug raw material and for assay of drug in tablets was developed. The method specifies a 3 jxm Hypersil nitrile column (150 × 4.6 mm), a mobile phase of 1 + 1 acetonitrile–ammonium acetate buffer (0.1 M adjusted to pH 6.0 with 0.1 M acetic acid), a flow rate of 1 mL/min, and detection at 240 nm. The lower limit of quantitation of the related compounds is 0.02% or less. Drug contents in 2 raw material samples were 100.1 and 99.9% and ranged from 98.2 to 99.4% in 3 tablet formulations. Impurity levels in 2 samples of raw material from different manufacturers were ca 0.4%. The presence of 3 of the known related compounds in these samples was confirmed by liquid chromatographymass spectrometry. The method applied to raw materials was evaluated by a second laboratory and found to be satisfactory.

scholarly journals Concurrent chromatographic determination of pseudoephedrine and loratadine from combination syrups and tablets

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Imad Osman Abu Reid
Keyword(s):  
Ammonium Acetate ◽  
Chemical Properties ◽  
Chromatographic Determination ◽  
Analytical Challenge ◽  
Intermediate Precision ◽  
Box Behnken Design ◽  
Complex Samples ◽  
System Suitability ◽  
Nonpolar Compounds

Abstract Background Chromatographic separation of polar and nonpolar compounds when presented in combined dosage forms has always been considered as great analytical challenge. Separation and retention of both polar and nonpolar compounds by the same stationary phase can be a useful approach for analyses of complex samples with such a difference in chemical properties. Loratadine (nonpolar) and pseudoephedrine (polar) are typical examples of this situation. Results The Box–Behnken design was used to optimize the separation process, an efficient separation of loratadine and pseudoephedrine was achieved within 6 min; employing a mixture of 16.0 mM ammonium acetate buffer (pH 4.5) and acetonitrile (23:77, v/v) as isocratic mobile phase, pumped at 1.0 mL/min through a Zorbax cyanopropyl column (250 mm × 4.6 mm, 5 μm), the analytes were detected at 250 nm. Under the same conditions, separation of sodium benzoate preservative co-formulated with the two analytes in syrup formulation was also achieved. The calibration curve demonstrated excellent linearity in the range of 24.6–123.2 μg/mL and 594.8–2974.0 μg/mL for loratadine and pseudoephedrine, respectively with determination coefficient (r2) > 0.999. Conclusion The method’s accuracy bias < 2.0%, repeatability and intermediate precision (%RSD < 2.0%) were verified. In addition, system suitability parameters were found within the acceptable limits. Satisfactory results were obtained upon the application of the validated method to the analysis of commercial tablet and syrup formulations.

Optimized liquid-chromatographic determination of metronidazole and its metabolites in plasma.

1984 ◽  
Vol 30 (5) ◽  
pp. 784-787 ◽  
Author(s):  
R A Gibson ◽  
L Lattanzio ◽  
H McGee
Keyword(s):  
Rapid Determination ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Detector Response ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Method ◽  
Wide Range ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Metronidazole and its known metabolites in plasma can be rapidly separated by a "high-pressure" liquid-chromatographic method that can also be adapted for rapid determination of tinidazole. Samples deproteinized with trichloroacetic acid (50 g/L final concentration) undergo isocratic separation on a reversed-phase C18 column eluted with an 8/92 (by vol) mixture of acetonitrile/KH2PO4 (5 mmol/L, pH 3.0). The method is sensitive, reliably detecting as little as 25 micrograms of metronidazole and (or) its metabolites per milliliter of plasma. The detector response varied linearly with concentration for all compounds tested over a wide range (25-500 micrograms/L). Within-day and between-day variation was generally less than 2.5% for all concentrations of all compounds tested. Various other antibiotics tested did not interfere.

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.

Liquid Chromatographic Determination of Diazepam in Tablets: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 545-546
Author(s):  
Michael Tsougros
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Photometric Detection ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
The Mean ◽  
Liquid Chromatographic

Abstract A stability indicating liquid chromatographic method for the determination of diazepam in tablets was collaboratively studied by 6 laboratories. The method uses a Cig reverse phase column, a methanolwater mobile phase, p-tolualdehyde as the internal standard, and photometric detection at 254 nm. The collaborators were supplied with a synthetic tablet powder and 3 commercial tablet samples. The mean recovery of diazepam from the synthetic tablet powder was 100.2%. For all samples analyzed, the coefficient of variation was &lt; 1.5%. The method has been adopted official first action.

Liquid Chromatographic Determination of Cinnamic and Benzoic Acids in Benzoin Preparations

1987 ◽  
Vol 70 (4) ◽  
pp. 689-691
Author(s):  
Abdel-Aziz M Wahbi ◽  
Mohammad A Abounassif ◽  
El-Rasheed A Gad-Kariem ◽  
Mahmoud W Ibrahim
Keyword(s):  
Chromatographic Determination ◽  
Cinnamic Acids ◽  
Reverse Phase ◽  
British Pharmacopoeia ◽  
Liquid Chromatographic Method ◽  
Individual Determination ◽  
Liquid Chromatographic Determination ◽  
The Individual ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for the individual determination of benzoic and cinnamic acids in 2 benzoin preparations is presented. The method specifies a reverse phase column and 0.01M KH2P04- methanol (85 + 15) as mobile phase at a flow rate of 1.8 mL/min, with detection at 254 nm. The method has been applied to 2 benzoin preparations and the results were compared with those from the British Pharmacopoeia method.

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