scholarly journals Determination of Monensin in High-Moisture Cattle Rations by Liquid Chromatography with Postcolumn Derivatization

1996 ◽  
Vol 79 (6) ◽  
pp. 1255-1259
Author(s):  
Debbie A Bridges ◽  
Doug M Roth ◽  
Christine M Cleveland ◽  
John W Moran ◽  
Mark R Coleman

Abstract An existing liquid chromatographic method using postcolumn derivatization has been used extensively to quantitate monensin in animal feeds. Because of the relatively high moisture content of many cattle feed rations, some modifications were made to this method. Several sample-processing steps were evaluated to determine optimum sample-processing procedure. The sample weight/sample diluent ratio was modified, and method linearity was validated for the lower monensin concentrations anticipated in high-moisture cattle rations. The accuracy and precision of data generated at these lower concentrations were also determined. Because of the high moisture content of these rations, data analysis for this method required correction of feed potency for loss on drying. With these modifications, monensin can be accurately determined in high-moisture cattle rations.

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.


2018 ◽  
Vol 101 (2) ◽  
pp. 401-409 ◽  
Author(s):  
Asmaa A El-Zaher ◽  
Ehab F Elkady ◽  
Hanan M Elwy ◽  
Mahmoud Abo El Makarim Saleh

Abstract A new LC method is introduced with the concept of its versatile application to widely used drugs from different pharmacological classes. Metformin hydrochloride (MTF), sitagliptin phosphate (SIT), simvastatin (SIM) and ezetimibe (EZB) were simultaneously determined with a simple reversed-phase LC method in which a SIT–SIM binary mixture, present in a dosage form brand, was considered central for its development. Chromatographic separation was achieved with a mobile phase of acetonitrile and 0.02 M potassium dihydrogen phosphate (pH 5.2) (77 + 23, v/v) flowing through a C18 column (BDS Hypersil, 250 × 4.6 mm, 5 µm) at 1.2 mL/min at ambient temperature. UV detection was programmed to be carried out at 210 nm for EZB, SIT, and MTF, whereas SIM was detected at 240 nm. The method was validated according to International Conference on Harmonization guidelines. Linearity, accuracy, and precision were satisfactory over concentration ranges 4–40 µg/mL for EZB and SIM, 0.5–50 µg/mL for SIT, and 5–500 µg/mL for MTF. Coefficients of determination were >0.99 for the four drugs. LOQs found were 0.01 µg/mL for EZB, 0.02 µg/mL for SIT, 0.2 µg/mL for MTF, and 0.02 µg/mL for SIM. The developed method is simple, rapid, accurate, precise, and suitable for the routine QC analysis of the cited drugs in pharmaceutical products by conventional HPLC systems.


1994 ◽  
Vol 77 (6) ◽  
pp. 1341-1346
Author(s):  
Hafez Abdel-Kader ◽  
Sylvia V Fagan ◽  
Govtnd K Menon ◽  
Larry S Wigman ◽  
Frederic Chapin

Abstract A rapid and sensitive 2-peak liquid chromatographic (LC) method is described for extracting and quantitating ardacin in premix, supplement, and animal feed formulations. Ardacin is extracted from the formulations and analyzed after dilution or cleanup by reversed-phase LC with UV detection at 220 nm. The method correlates well with a more information-rich gradient multipeak LC method. Recoveries for premix formulations ranged from 96.8% (relative standard deviation [RSD], 0.8%) to 103.7% (RSD, 1.3%) for laboratory samples spiked at levels ranging from 1.6 to 39.6% ardacin. Recoveries for protein supplement mash formulations ranged from 98.7% of claim (RSD, 4.1%) to 106.0% of claim (RSD, 7.7%) at ardacin levels ranging from 37.5 to 600 mg/lb. Recoveries for cattle feed ranged from 90.0% of claim (RSD, 11.9%) to 105.6% of claim (RSD, 2.7%) at ardacin levels ranging from 4 to 30 g/ton.


2010 ◽  
Vol 7 (1) ◽  
pp. 260-264 ◽  
Author(s):  
V. V. Vaidya ◽  
G. R. Singh ◽  
M. P. Choukekar ◽  
M. B. Kekare

A simple, fast and precise reverse phase high performance liquid chromatographic method is developed for the simultaneous determination of aceclofenac, paracetamol and tizanidine. Chromatographic separation of the three drugs were performed on a hypersil C18column (250 mm x 4.6 mm, 5 µm) as stationary phase with a mobile phase comprising of mix phosphate buffer pH 7.0: acetonitrile (40:60 v/v), at a flow rate of 0.7 mL min-1and UV detection at 230 nm. The proposed method was validated for linearity, accuracy, precision, LOD, LOQ. Linearity, accuracy and precision were found to be acceptable over the ranges of 100-300 µg mL-1for aceclofenac, 500-1500 µg mL-1for paracetamol and 2-6 µg mL-1for tizanidine HCl equivalent to tizanidine. It can be conveniently adopted for routine quality control analysis.


2012 ◽  
Vol 31 (1) ◽  
pp. 47 ◽  
Author(s):  
Natalija Nakov ◽  
Jelena Acevska ◽  
Katerina Brezovska ◽  
Rumenka Petkovska ◽  
Aneta Dimitrovska

A new Hydrophilic Interaction Liquid Chromatography (HILIC) method was developed for simultaneous determination of cetylpyridinium chloride and benzocaine as active substances in lozenges. Method development included investigation of the influence of the critical chromatographic conditions such as: type of organic modifier, mobile phase strength, ionic strength and pH value of the buffer used in the mobile phase, as well as experimental determination of dominant mechanism of retention. The optimal chromatographic conditions were obtained using bare silica column and a mobile phase consisting of acetonitrile and ammonium formate (50 mM, pH = 4.0) in ratio 80 : 20 V/V. The method was validated in terms of specificity, linearity, accuracy and precision. The validation results indicate that the proposed HILIC method is suitable for quantitative analysis of cetylpyridinium chloride and benzocaine in lozenges.


2006 ◽  
Vol 49 (spe) ◽  
pp. 41-46 ◽  
Author(s):  
Roseane Brandão de Brito ◽  
Roberto Gonçalves Junqueira

A high performance liquid chromatographic method to assay beta-lactam residues in milk was developed and validated. Milk samples were spiked with standard solutions and deproteinated. The extract was cleaned-up on C18 SPE cartridge, the antibiotics eluted with acetonitrile:water (50:50 v/v) and derivatized with acetic anhydride and 1-methyl-imidazole solution containing HgCl2. The chromatographic analysis was performed on C18 column using mobile phase consisting of acetonitrile and phosphate buffer (pH 6.5) in the presence of Na2S2O3 gradient and detection at 325 nm. The method was selective for ampicillin, penicillin G and penicillin V, the latter used as internal standard. Average recoveries for ampicillin and penicillin G ranged, respectively, from 60.0% to 104.9% and from 82.7% to 109.2%, with coefficients of variation from 11.1% to 24.6%, and from 2.1% to 25.2%, indicating accuracy and precision. Detection limit of 4.0 µg/L for ampicillin and 3.0 µg/L for penicillin G, and quantification limits of 4.0 µg/L for both were estimated.


1993 ◽  
Vol 76 (5) ◽  
pp. 1027-1032 ◽  
Author(s):  
M L Izquierdo-Pulido ◽  
M C Vidal-Carou ◽  
A Marine-Font

Abstract A liquid chromatographic method is described for the determination in one run of the following 10 biogenic amines in beers: histamine, tyramine, serotonin, (β-phenylethylamine, tryptamine, cadaverine, putrescine, agmatine, spermine, and spermidine. The method is based on ion-pair chromatographic partition on a reversed-phase column and involves a postcolumn reaction with o-phthalaldehyde (OPT) to form fluorescent derivatives with amines. Treatment of beer samples before injection requires only a filtration through a 0.45 μm filter. It is necessary to obtain a perchloric extract for analysis of raw materials (malt and hops). The method was tested for lack of interference from amino acids and other amines. Linearity, precision, recovery, and sensitivity were satisfactory. Detection limits ranged from 0.30 to 0.40 mg/L, and determination limits ranged from 0.40 to 0.50 mg/L, except for serotonin and spermine, which were slightly higher. The simple preparation of sample and the automatic accomplishment of derivatization steps considerably reduce analysis time and effort.


1995 ◽  
Vol 78 (4) ◽  
pp. 1045-1050 ◽  
Author(s):  
María Teresa Veciana-Nogues ◽  
Teresa Hernandez-Jover ◽  
Abel Marine-Font ◽  
María Del Carmen Vedal-Carou

Abstract A liquid chromatographic method with postcolumn derivatization is described for determination of biogenic amines in fish and fish products. Histamine, tyramine, serotonin, β-phenylethylamine, tryptamine, putrescine, cadaverine, agmatine, spermine, and spermidine can be determined in less than 60 min. Routine sample preinjection treatment implies only 2 extractions with 0.6N perchloric acid and filtration through a 0.45 μm filter. Lack of interferences from volatile amines, amino acids, and dipeptides was verified. Results of reliability study were satisfactory. The proposed method was linear for each amine between 0.25 and 8.00 mg/L. Average recoveries ranged from 92 to 103%. Precisions (coefficients of variation) ranged from 0.70 to 9.75%. Determination limits were ≤1 mg/kg. A modification in LC conditions was necessary to apply the method to ripened fish products to avoid interferences from food matrixes. In addition, stability of biogenic amines in fresh anchovies and hake during short-term frozen storage was studied. Results showed that, except for agmatine, frozen storage is suitable for keeping samples before analysis.


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