scholarly journals HPLC-DAD multi-residue method for determination of florfenicol, penicillin and tetracycline residues in raw cow milk

2021 ◽  
Vol 2 (3) ◽  
pp. 01-08
Author(s):  
Ali Jaber ◽  
Zeinab Zahreddine ◽  
Simon Abou Haidar ◽  
Chadi Hosri ◽  
Ghassan Ibrahim ◽  
...  
Keyword(s):  
High Performance ◽  
Solid Phase ◽  
Raw Milk ◽  
Reversed Phase ◽  
Cow Milk ◽  
Antibiotic Residues ◽  
Milk Samples ◽  
Antibiotics Residues ◽  
Tetracycline Residues

The existence of antibiotic residues in edible products constitutes a health problem to the consumers. Reversed-phase high-performance liquid chromatography with diode array detection (HPLC–DAD) was optimized and validated for the simultaneous determination of florfenicol (FF), penicillin (PE), and tetracycline (TC) residues in dairy raw milk samples. The determination of these antibiotics was carried out on HP-ODS Hypersil C18 (5μm, 125*4 mm) column at a flow rate (1mL/min) and temperature (35 ⁰C). The extraction method includes deproteinization of the milk sample followed by a solid-phase extraction (SPE) clean-up. The method was validated according to the European Commission Decision 2002/657/EC and the International Conference of Harmonization Guidelines. The recoveries for the studied antibiotics ranged from 82–111.54 % making the method suitable for performing routine analysis. The proposed method was applied for the analysis of antibiotic residues in 50 dairy raw milk samples collected from many regions in Lebanon. The results showed the occurrence of these antibiotics residues in milk collected from different Lebanese regions. The numbers indicate that 22 % of milk samples were found to be positive for FF, 42 % for PE, and 28 % for TC residues.

scholarly journals βeta-lactam and Tetracycline Antibiotic Residues in Cow Milk in the Constantine region, Algeria

2021 ◽  
Vol 53 (3) ◽  
Author(s):  
Noureddine Zeghilet ◽  
Brahim Bouchoucha ◽  
Omar Bouaziz
Keyword(s):  
Milk Sample ◽  
Dairy Industry ◽  
Raw Milk ◽  
Control Programme ◽  
Cow Milk ◽  
Antibiotic Residues ◽  
Pasteurized Milk ◽  
Tetracycline Antibiotic ◽  
Milk Samples ◽  
Antibiotics Residues

The aim of the present study was to investigate the βeta-lactam and tetracycline antibiotic residues in cow milk samples. A total of 122 samples of cow milk were collected from raw milk collectors (109 samples) and from a reconstituted pasteurized milk sales clerk (13 samples) in the Constantine region, Algeria and examined using the ΒetaStar Combo screening kit (Neogen, USA). Results indicates that 13 samples (10.66%) were positive for antibiotics residues: 12 (9.84%) for βeta-lactams (ten (8.20%) raw and two (1.64%) pasteurized milk samples) and only one (0.82%) for tetracyclines in a raw milk sample. It is evident that the Algerian consumer is not sheltered from the danger of antibiotic residues in milk and these inhibitor residues should constitute a constant concern for the dairy industry in Algeria. A control programme should be established.

scholarly journals Detection of antibiotic residues in locally raw milk by using high performance liquid chromatography at different seasons and the effect of heat treatment on their concentration

2018 ◽  
Vol 41 (2) ◽  
pp. 131-136
Author(s):  
Ahmed Salman Moqef Al- kurashi
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Bovine Milk ◽  
Raw Milk ◽  
Antibiotic Residues ◽  
Milk Samples ◽  
Bulk Milk ◽  
Antibiotics Residues ◽  
High Degree

     The aim of this study was to determine the level of antibiotics residues in the locally produced cows raw milk as well as to evaluate the effect of different commercial heat treated process on the level of antibiotics residues in milk. A total of 52 locally produced milk samples were collected from apparently healthy cows in AL-Fudhailia village, milk cans (50 Kg), bulk milk tanks (1, 5 and 10 tons) which belonged to the milk reception and collection centers and dairy plants in Baghdad were collected during beginning of December 2015 to the end of April 2016. Results revealed by using high performance liquid chromatography that there was a significant seasonal variation in the residual concentration of each detected antibiotic in milk samples, where it was found that all cow's milk samples had significantly higher concentrations of antibiotic residues in spring than in winter seasons. Generally by excluding both the season and the kind of antibiotic, it was found that milk samples that were collected from 50 Kg milk cans recorded significantly highest antibiotic residues followed by bulk milk tanks of 1 and 5 tons in comparison to 10 tons. Antibiotics recovery experiment was conducted by spiking the bovine milk samples with Known concentrations four ß-lactams (Benzylpencillin, Cloxacillin, Amoxcilin, Ampcilline) and other five detected antibiotics and then exposed to one of the three different commercial heat treatments. The results showed that the pasteurization process (63°C/30 min.) a slight inactivation of four ß-lactams and other five detected antibiotics, whereas 80°C/5 min. high degree of antimicrobial loss at the rate of 89% and 82%. However, boiling at 100°C/5 min, high degree of antimicrobial loss at the rate of 100% and 90% respectively.

scholarly journals Determination of Flumorph Residues in Vegetables, Soil, and Natural Water by Solid-Phase Extraction Cleanup and High-Performance Liquid Chromatography with UV Detection

2008 ◽  
Vol 91 (6) ◽  
pp. 1459-1466 ◽  
Author(s):  
Ji-Ye Hu ◽  
Yu-Chao Zhang ◽  
Hai Yan
Keyword(s):  
Solid Phase Extraction ◽  
Natural Water ◽  
High Performance ◽  
Solid Phase ◽  
Residue Analysis ◽  
Reversed Phase ◽  
Uv Detection ◽  
Phase Extraction ◽  
Limit Of Quantification

Abstract A method for high-performance liquid chromatographic (HPLC) determination of flumorph residues in cucumber, tomato, soil, and natural water was developed and validated. Primary secondary amine or octadecylsilyl (C18) solid-phase extraction cartridges were used for sample preparation. Reversed-phase HPLC with UV detection was used for separation and quantification of the pesticide. The combined cleanup and chromatographic method steps were sensitive and reliable for simultaneous determination of residues of the 2 isomers of flumorph in the studied samples. This method is characterized by recovery >97.9, coefficient of variation <6.2, and limit of quantification of 0.01 mg/kg, in agreement with directives for method validation in residue analysis. Flumorph residues in the samples were further confirmed by HPLC/mass spectrometry. The proposed method is fast, easy to perform, and could be used for monitoring of pesticide residues.

scholarly journals Determination of Four Fluoroquinolones in Milk by Liquid Chromatography

1997 ◽  
Vol 80 (5) ◽  
pp. 982-987 ◽  
Author(s):  
José E Roybal ◽  
Allen P Pfenning ◽  
Sherri B Turnipseed ◽  
Calvin C Walker ◽  
Jeffrey A Hurlbut
Keyword(s):  
Fluorescence Detection ◽  
Solid Phase ◽  
Raw Milk ◽  
Extraction Column ◽  
Isocratic Elution ◽  
Standard Curve ◽  
Milk Samples ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method with fluorescence detection is presented for the analysis of 4 fluoroquinolones; enrofloxacin (ENRO), ciprofloxacin (CIPRO), sarafloxacin (SARA), and difloxacin (DIFLX) in milk. The procedure consists of extraction of milk with acidified ethanol, isolation and retention on a cation exchange solid-phase extraction column, elution with basic methanol, and LC analysis with fluorescence detection. LC analysis is performed by isocratic elution using an acetonitrile-2% acetic acid (15 + 85) mobile phase and an Inertsil phenyl column with fluorescence detection at excitation and emission wavelengths of 278 and 450 nm, respectively. A target level of 10 ppb for each of the 4 fluoroquinolones has been established for this method. Average recovery from fortified raw milk samples (5-100 ppb each) based on a 5-point standard curve calculation was 70-90%, with relative standard deviations of <15%.

Dispersive Micro-Solid Phase Extraction Combined with High-Performance Liquid Chromatography for the Determination of Three Penicillins in Milk Samples

2014 ◽  
Vol 8 (5) ◽  
pp. 1079-1087 ◽  
Author(s):  
Noorfatimah Yahaya ◽  
Mohd Marsin Sanagi ◽  
Takahito Mitome ◽  
Norikazu Nishiyama ◽  
Wan Aini Wan Ibrahim ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
High Performance ◽  
Solid Phase ◽  
Phase Extraction ◽  
Milk Samples

scholarly journals Multiresidue Analytical Method for the Determination of Eight Penicillin Antibiotics in Muscle Tissue by Ion-Pair Reversed-Phase HPLC after Precolumn Derivatization

1999 ◽  
Vol 82 (5) ◽  
pp. 1083-1095 ◽  
Author(s):  
Eric Verdon ◽  
Pierrick Couëdor
Keyword(s):  
Muscle Tissue ◽  
Phosphate Buffer ◽  
High Performance ◽  
Solid Phase ◽  
Sodium Thiosulfate ◽  
Reversed Phase ◽  
Extraction Column ◽  
Precolumn Derivatization ◽  
Solution Ph

Abstract A high-performance liquid chromatographic multiresidue method was developed for the determination of 8 penicillin compounds (benzylpenicillin, phenoxymethylpenicillin, ampicillin, amoxicillin, nafcillin, oxacillin, cloxacillin, and dicloxacillin) at trace levels in muscle tissue. This method involves extraction of the penicillins with phosphate buffer pH 9 followed by cleanup and concentration on a C18 solid¯phase extraction column and reaction with benzoic anhydride at 50°C for 5 min and with 1,2,4-triazole and mercury(II) chloride solution pH 9 at 65°C for 10 min. The derivatized compounds are eluted on a C18 column with a mobile phase containing acetonitrile and phosphate buffer (pH 6; 0.1 mol/L) loaded with sodium thiosulfate and ion-pairing tetrabutylammonium hydrogenosulphate. The method detection limit is approximately 3-11 μg/kg and the limit of determination was evaluated down to 25 μg/kg in line with the criteria of the EU decision No. 93/256/EEC.

Detection of trace amounts of abamectin used as an antiparasitic agent in fallow deer tissues

2009 ◽  
Vol 57 (1) ◽  
pp. 99-107 ◽  
Author(s):  
Diana Žele ◽  
Silvestra Kobal ◽  
Gorazd Vengušt ◽  
Andrej Bidovec ◽  
Anton Vengušt ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Fallow Deer ◽  
Reversed Phase ◽  
Fat Tissue ◽  
Matrix Interference ◽  
Solid Phase Extraction Cartridge ◽  
Tissue Matrix

A sensitive and reliable method for the determination of trace amounts of abamectin in muscles, kidneys and fat tissue of fallow deer is presented. Abamectin was extracted from the tissues with acetonitrile and the extract was cleaned up on a C8 solid-phase extraction cartridge. Abamectin residue was derivatised with trifluoroacetic acid anhydride and 1-methylimidazole, and determined using reversed- phase high-performance liquid chromatography under isocratic conditions and fluorescence detection. The recoveries of the method were high and consistent, ranging from 78% to 90%. The limit of detection of the method was below 1 μg/kg when analysing muscle, kidney and fat tissue. Matrix-matched calibration was used in order to obtain accurate values and to avoid matrix interference.

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