Comparison of Sulfadimethoxine Residue Analyses in Salmon Muscle Using HPLC and Charm II Test

1995 ◽  
Vol 58 (6) ◽  
pp. 678-682 ◽  
Author(s):  
DAVID D. KITTS ◽  
MING ZHENG ◽  
ERIN BURNS-FLETT ◽  
KEITH M. McERLANE

Sulfadimethoxine (SDM) residues in chinook salmon muscle were measured by high-performance liquid chromatography (HPLC) and the Charm II test to evaluate the efficacy of the Charm test for the measurement of sulfonamide residues in fish muscle. Both HPLC and Charm analyses were performed in the presence of salmon tissue matrix for the purpose of evaluating the results in field conditions. The sensitivity of the HPLC method was 0.05 μg/g (0.05 ppm) for SDM, while the sensitivity of the Charm II test was at least 0.01 ppm. SDM analysis from salmon fed Romet-30® performed using the Charm assay gave consistently lower values compared to HPLC; however, good agreement was obtained between both methods (r2 = 0.944) over a concentration range of 0.1 to 13.0 ppm in muscle tissue. The large variation in SDM concentrations between fish sampled on common days suggests that a larger number of fish are required for more accurate risk assessment. In the current investigation, the Charm II test was shown to be effective in measuring SDM in salmon muscle tissue for the large sample throughput common with antibiotic-screening strategies.

2011 ◽  
Vol 94 (2) ◽  
pp. 446-452 ◽  
Author(s):  
Donglei Yu ◽  
Nathan Rummel ◽  
Badar Shaikh

Abstract An HPLC method was developed for the determination of albendazole (ABZ) and its metabolites, a sulfoxide (ABZSO), a sulfone (ABZSO2), and albendazole-2-aminosulfone (ABZ-2-NH2SO2), from yellow perch muscle tissue with adhering skin. The muscle tissue samples were made alkaline with potassium carbonate and extracted with ethyl acetate, followed by a series of liquidliquid extraction steps. After solvent evaporation, the residue was reconstituted in the initial mobile phase combination of the gradient. The mobile phase consisted of a buffer, 50 mM ammonium acetate (pH 4.0) in 10 methanolwater, and 100 acetonitrile. The gradient was from 20 acetonitrile to 85 acetonitrile. The analytes were chromatographed on an RP Luna C18(2) column and detected by fluorescence with excitation and emission wavelengths of 290 and 330 nm, respectively. The average recoveries from fortified muscle tissue for ABZ (20100 ppb), ABZ-SO (20200 ppb), ABZSO2 (8100 ppb), and ABZ-2-NH2SO2 (20100 ppb) were 85, 95, 101, and 86, respectively, with corresponding CV values of 9, 3, 6, and 4, respectively. Their LOQ values were 10, 10, 1, and 10 ppb, respectively. The procedure was applied to determine ABZ and its major metabolites in the incurred muscle tissue of yellow perch obtained after orally dosing the fish with ABZ.


1999 ◽  
Vol 82 (5) ◽  
pp. 1097-1101 ◽  
Author(s):  
Guillaume Duflos ◽  
Catherine Dervin ◽  
Pierre Malle ◽  
Stephane Bouquelet

Abstract Spoilage can be evaluated by separating and determining biogenic amines by various techniques, notably high-performance liquid chromatography. Previous studies have not taken into account how the muscle tissue matrix affects the assay. We demonstrate a matrix effect in plaice and whiting and show that it changes during spoilage. This effect should be taken into account when plotting regression lines relating the quantity of amine to the biogenic amine/internal standard ratio.


2018 ◽  
Vol 10 (5) ◽  
pp. 167 ◽  
Author(s):  
Ahmed Mahdi Saeed ◽  
Mohammed Jassim Hamzah ◽  
Noor Qasim Ahmed

Objective: Easy and precise methods were developed for estimation of aspirin (ASP), impurities from such as salicylic acid (SAL) and heavy metal ions (HMI) in ASP tablets that available in the Iraqi’s market using High-performance liquid chromatography (HPLC), UV–VIS spectrophotometry and atomic absorption spectrophotometric (AAS).Methods: HPLC separation was carried out using C18 as stationary phase and acetonitrile (ACN): water in the ratio of (10: 90 v/v) as a mobile phase for HPLC method and as a solvent for UV-VIS spectrophotometric for quantitative ASP and SAL at 254 nm for HPLC, 226 and 296 nm for UV measurements. AAS was used for HMI determination.Results: ASP and SAL gave absorbance maxima at 226 and 296 nm in ACN: H2O solvent. The Beer’s law was obeyed in the range of 0.05-20 for ASP and 0.02-8 µg/ml for SAL. Correlation coefficients (R2) were 0.9996 and 0.9992 for ASP and SAL respectively, for HPLC and LOD value was 0.006 for ASP and 0.004 μg/ml for SAL. The % recovery for the developed method was found to be in the range of (98.80 to 101.26%) and (98.67 to 103.33%) for ASP and SAL respectively, within the acceptable range, that approved by world health organization (WHO).Conclusion: The proposed method can help research studies, quality control and routine analysis with lesser resources available. The results of the assay of pharmaceutical formulation of the developed method are highly reliable and reproducible and is in good agreement with the label claim of the medicines.


Author(s):  
B G Keevil ◽  
P W Maylor ◽  
D Rowlands

We developed a binary gradient high-performance liquid chromatography (HPLC) method for measuring HbA2 in whole blood samples using a Pharmacia Mono Q column (1 mL) and measurement at 415 nm. The assay requires a simple lysis and centrifugation step before injection onto the column. We found good agreement of results between the HPLC method and the Helena column chromatography method. The within batch precision was 2·6% and between batch precision was 4·6%. We found that using 30 mM Tris buffers (pH 7·8) with a sodium chloride gradient resulted in short analysis times and good chromatographic separation of HbA2, HbS and HbA. We conclude that this is a robust assay for the diagnosis of β-thalassaemia.


2019 ◽  
Vol 31 (11) ◽  
pp. 2473-2478
Author(s):  
Kadali Jagadeesh ◽  
Nowduri Annapurna

This study reports a new stability indicating HPLC method using Spursil C18 column as stationary phase, and mixture of 0.1 M Na2HPO4 and methanol (50:50 v/v) as mobile phase for the chromatographic determination of paracetamol and prochlorperazine in tablets and in bulk form. The linearity range is 250-750 μg/mL for paracetamol and 2.5-7.5 μg/mL for prochlorperazine. The limit of detection values are 2.650 μg/mL for paracetamol and 0.175 μg/mL for prochlorperazine. The minor values of the relative standard deviation (≤ 2.0 %) as well as good percent assay values (nearer to 100 %) confirm the high precision and accuracy of the present method. From the degradation study chromatograms found that there was no interference from degradants when paracetamol and prochlorperazine are quantified in tablets through the proposed method. A good agreement between results obtained and labeled claim for the determination of paracetamol and prochlorperazine in tablet samples demonstrates that the proposed method is appropriate to quantify paracetamol and prochlorperazine in tablet formulations.


Author(s):  
Arun Kumar P. ◽  
Elangaimannan R.

The study was conducted to evolve Gloriosa superba for yield characters and alkalodi content for selecting elite genotypes for comercial exploitatio n. The genotypes were sowm in Variyankaval village, Udayarpalayam taluk of Ariyalur district, Tamil Nadu. The highest mean value for fresh and dry seed yield was observed in Chittor local. The genotype Mulanur local has recorded the highest mean value for number of pods per plant and number of seeds per pod and Arupukotai local excelled the general mean for the traits seeds per pod, fresh and dry seed yield and also for tuber characters. An investigation was carried out to quantify the colchicine (alkaloid) present in tubers by High Performance Liquid Chromatography (HPLC) method. The genotypes collected from Arupukotai recorded the highest colchicine content (0.760 mg/g) followed by Chittoor (0.578 mg/g) and Mulanur (0.496 mg/g) and there by these three genotypes were utilized for further crop improvement.


2020 ◽  
Vol 20 (13) ◽  
pp. 1053-1059
Author(s):  
Mahmoud M. Sebaiy ◽  
Noha I. Ziedan

Background: Allergic diseases are considered as the major burden on public health with increased prevalence globally. Histamine H1-receptor antagonists are the foremost commonly used drugs in the treatment of allergic disorders. The target drug in this study, loratadine, belongs to this class of drugs and its biometabolite desloratadine which is also a non-sedating H1 receptor antagonist with anti-histaminic activity being 2.5 to 4 times greater than loratadine. This study aimed to develop and validate a novel isocratic Reversed-phase High-Performance Liquid Chromatography (RP-HPLC) method for rapid and simultaneous separation and determination of loratadine and its metabolite, desloratadine in human plasma. Methods: The drug extraction method from plasma was based on protein precipitation technique. The separation was carried out on a Thermo Scientific BDS Hypersil C18 column (5μm, 250 x 4.60 mm) in a mobile phase of MeOH: 0.025M KH2PO4 adjusted to pH 3.50 using orthophosphoric acid (85: 15, v/v) at an ambient temperature. The flow rate was maintained at 1 mL/min and maximum absorption was measured using the PDA detector at 248 nm. Results: The retention times of loratadine and desloratadine in plasma samples were recorded to be 4.10 and 5.08 minutes, respectively, indicating a short analysis time. Limits of detection were found to be 1.80 and 1.97 ng/mL for loratadine and desloratadine, respectively, showing a high degree of sensitivity of the method. The method was then validated according to FDA guidelines for the determination of the two analytes in human plasma. Conclusion: The results obtained indicate that the proposed method is rapid, sensitive in the nanogram range, accurate, selective, robust and reproducible compared to other reported methods.


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