Determination of Fluoroquinolones Residual in Freshwater Fish by HPLC

2014 ◽  
Vol 1033-1034 ◽  
pp. 634-637
Author(s):  
Yue Jin ◽  
Wen Yu Zhang ◽  
Qian Wang ◽  
Yi Qing Yang ◽  
Li Ya Liang ◽  
...  

HPLC (High Performance Liquid Chromatography) method for danofloxacin(DAN), enrofloxacin(ENR), sarafloxacin(SAR) and difloxacin(DIF) residues in freshwater fish was developed. The fish sample was extracted with methanol-water-acetic acid(2/8/0.01, V/V/V), performed on a C18 solid-phase extraction column. With methanol+malonic acid-magnesium chloride aqueous solution as mobile phase, gradient elution at 30°C, inject volume was 20μL. The wavelength of UV detector was 280 nm. The linear rang of four drugs was 0.1~10μg/mL. In the level of 0.5μg/kg and 4.0μg/kg, the average recovery of the four kinds of drugs was 79.81%~92.03% , the RSD was 1.03%~4.07%. The limit of DAN, ENR, SAR, and DIF was 0.1μg/kg, 0.1μg/kg, 0.05μg/kg, and 0.05μg/kg individual. This method was employed to analyze freshwater fishes, such as catfish, chub and carp, because of its simplicity and high efficiency.

2012 ◽  
Vol 56 (3) ◽  
pp. 329-333 ◽  
Author(s):  
Ewelina Patyra ◽  
Ewelina Kowalczyk ◽  
Krzysztof Kwiatek

Abstract High performance liquid chromatography method with diode array detection (HPLC-DAD) was developed and optimised for the determination of tetracyclines (TCs) in medicated feedingstuffs. The extraction of the analyte from feedingstuffs was performed with Na2EDTA-McIlvaine buffer (pH 2.5 and pH 4). The extracts were cleaned up by solid phase extraction using octadecyl cartridges (C18). The samples were dried up and redissolved in the mixture of oxalic acid and methanol. Separation was performed on reserved phase column (Phenomenex C18, 250 x 4.6 mm, 5 μm) by multistep gradient elution, which provided better chromatographic separation. The analysis was performed at a wavelength of 390 nm. Validation study of the method revealed that all obtained calibration curves showed good linearity R= 0.9985 for doxycycline (DC) and R= 0.9981 for chlorotetracycline (CTC) over the range of 25-2,000 mg/kg. The analytical procedure was successfully adapted for quantitative determination of DC and CTC in medicated feedingstuff samples. Validation included determination of specificity, linearity, and repeatability. Mean recovery for spiked samples was 93.1% for CTC and 93.2% for DC. The results of validation of the analytical procedure proved that presented method is efficient, precise and useful for quantification of DC and CTC in medicated feedingstuffs.


2012 ◽  
Vol 503-504 ◽  
pp. 289-292
Author(s):  
Hong Yuan Yan ◽  
Zhi Wei Li ◽  
Jing Yu Zhang ◽  
Chang Qing He

Two kinds of triazine herbicides (cyanazine and atrazine) in cucumber were analyzed by high performance liquid chromatography method coupled with pseudo imprinted solid-phase extraction (PISPE) as the clean-up arrays. The sorbent of PMISPE was synthesized by bulk polymerization using cyromazine as pseudo template and it could selectivly recognized cyanazine and atrazine from cucumber matrix. The mobile phase for separation and quantity analysis of cyanazine and atrazine was methanol-(0.8% acetic acid-water) (55:45, v/v) with a UV detector being set at 224 nm. The result showed that good linearity of the two trazine herbicides was obtained in a range of 0.004 µg/g ~ 0.400 µg/g with r2≥0.9996 and the recoveries at three spiked levels were ranged from 93.8% to 108.5% with RSD less than 3.4% (n=3).


2011 ◽  
Vol 29 (No. 6) ◽  
pp. 641-646 ◽  
Author(s):  
P. Navrátilová ◽  
I. Borkovcová ◽  
J. Vyhnálková ◽  
L. Vorlová

The aim of the study was to monitore the levels of fluoroquinolone residues in bulk samples of raw cow’s milk. The bulk samples of raw cow’s milk (n = 150) were obtained from 58 different milk suppliers in the South Moravian and Vysočina Regions. The samples were analysed by reverse phase high-performance liquid chromatography method with fluorescence detection and gradient elution. 87.3% of the raw milk samples were positive for the fluoroquinolones residues. Flumequine was present in none of the samples. The levels of other fluoroquinolones investigated were below the recommended maximum residue limit. The results of the study indicate that fluoroquinolones are frequently administered to the dairy cows in spite of the recommendations of CVMP. The most frequently determined was enrofloxacin and its indicator residue, i.e. ciprofloxacin. An efficient control of the veterinary drugs residues in milk is very important to ensure the safety of the milk and milk products.


2013 ◽  
Vol 340 ◽  
pp. 388-391 ◽  
Author(s):  
Xiang Ke Cao ◽  
Qing Zeng Qian ◽  
Jun Wang Tong ◽  
Qian Wang

By solid - phase extraction high performance liquid chromatography determination of nonylphenol, Octylphenol in aquatic product residues, to establish more accurate, fast, effective detection method. Sample is 3 trichloroacetic acid solution after extraction, using anion exchange solid phase extraction column purification by reversed phase high performance liquid chromatography method for determination. Column is Shim-pack VP-ODS 250mm x4.6mm, detection wavelength is225 nm, mobile phase of methanol - water ( volume ratio of 75:25), flow rate is 0.8 mL/min, injection volume is 20 ìL. Octylphenol, nonylphenol respectively in 0.14¡«97.63 ìg/mL ( R=0.9995),0.02¡«51.04 ì g/mL ( R=0.9997) concentration and peak area show a good linear relationship, octylphenol nonylphenol and the recovery is 87.9%¡«93.8%, relative standard deviation is 1.4%¡«3.8%. Solid - phase extraction high performance liquid chromatography method for determination of aquatic product of octylphenol and nonylphenol residue is accurate, rapid, high sensitivity, suitable for aquatic products of octylphenol nonylphenol and detection.


2015 ◽  
Vol 78 (1) ◽  
pp. 151-156 ◽  
Author(s):  
L. S. YU ◽  
F. LIU ◽  
H. WU ◽  
H. R. TAN ◽  
X. C. RUAN ◽  
...  

A method for detection of flumethrin residue in honey by high-performance liquid chromatography was established. After n-hexane–dichloromethane (4:6, vol/vol) extraction, the honey samples were concentrated by rotary evaporation, purified by an Oasis HLB solid-phase extraction column, and detected using a UV detector at 267 nm. The interference of the matrix was greatly reduced by optimizing pretreatment conditions; thus, the minimal detection limit of cyhalothrin was 0.005 mg/kg, the average recovery was 80.8 to 96.8%, and the coefficient of variation was 0.6 to 1.5%. The precision and reproducibility of this method was suitable and applicable for detecting flumethrin residue in honey. With this method, 135 honey samples from seven locations in the People's Republic of China were tested; 77 samples tested positive for flumethrin residue, resulting in a detection rate of 75.3%. Samples from the Guangdong province had the highest flumethrin residue level (0.122 mg/kg) of the locations tested. On the basis of analytical validation, the high-performance liquid chromatography has been shown to be a promising alternative for the analysis of flumethrin residue in honey samples.


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