Rapid determination of glyphosate in cereal samples by means of pre-column derivatisation with 9-fluorenylmethyl chloroformate and coupled-column liquid chromatography with fluorescence detection

1999 ◽  
Vol 833 (1) ◽  
pp. 67-73 ◽  
Author(s):  
E.A. Hogendoorn ◽  
F.M. Ossendrijver ◽  
E. Dijkman ◽  
R.A. Baumann
2010 ◽  
Vol 93 (4) ◽  
pp. 1331-1339 ◽  
Author(s):  
Maki Kanda ◽  
Tomoto Kusano ◽  
Setsuko Kanai ◽  
Hiroshi Hayashi ◽  
Yoko Matushima ◽  
...  

Abstract A rapid and efficient method was developed for the simultaneous determination of seven fluoroquinolone (FQ) residues: norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, orbifloxacin, sarafloxacin, and difloxacin in honey. The samples were first screened with a microbiological method by using test plates made from metal-free purified agar seeded with Bacillus subtilis BGA. When a sample was found to contain FQ residues by using the microbiological method, it was analyzed by LC with fluorescence detection (LC/FL). FQs were extracted with Na2EDTA-McIlvaine buffer and purified by a dual SPE method in which a cation-exchange cartridge was connected to an anion-exchange cartridge. The overall recoveries of the seven FQs ranged from 70.0 to 92.1. The intra-assay and interassay CVs were 7.8 and 5.1, respectively. For the microbiological method, the LOD values ranged from 2 to 9 g/kg. For LC/FL, the LOQ values ranged from 2 to 7 g/kg. The developed method was used to analyze 70 honey samples. In 14 samples in which the microbiological method detected the presence of FQ residues, norfloxacin, ciprofloxacin, and enrofloxacin were identified by LC/FL.


2000 ◽  
Vol 83 (1) ◽  
pp. 17-19 ◽  
Author(s):  
Shozo Horii ◽  
Naoto Oku

Abstract A procedure was developed to determine nosiheptide residues in marketed meat and egg. Acetonitrile was used for the extraction, and the extract was partitioned with hexane to remove fat. The lower layer was reconstructed and quantitated by liquid chromatography using fluorescence detection at 357 nm excitation and 500 nm emission. The mobile phase consisted of 0.025% phosphoric acid–acetonitrile (50 + 50, v/v). Recoveries of nosiheptide from fortified samples ranged from 91.3 to 95.2% for swine muscle, 88.6 to 92.7% for chicken muscle, and 86.3 to 86.8% for egg. The method was used to monitor swine and chicken muscle and egg (20 samples each) in the market. Nosiheptide was not determined in all 60 samples.


2010 ◽  
Vol 666 (1-2) ◽  
pp. 38-44 ◽  
Author(s):  
P. Parrilla Vázquez ◽  
M. Martínez Galera ◽  
A. Serrano Guirado ◽  
M.M. Parrilla Vázquez

2004 ◽  
Vol 87 (2) ◽  
pp. 411-416 ◽  
Author(s):  
Roswitha Göbel ◽  
Klaus Lusky

Abstract The simultaneous determination of mycotoxins was performed in 3 steps: extraction, cleanup, and detection. For extraction, a mixture of acetonitrile–water (60 + 40, v/v) was proved appropriate. For cleanup, a new Afla-Ochra-Zea immunoaffinity column was used. After derivatization with trifluoroacetic acid, the mycotoxins aflatoxins, ochratoxin A (OTA), and zearalenone (ZEA) were determined simultaneously by liquid chromatography with fluorescence detection. The detection limits in different matrixes after cleanup with the new immunoaffinity column were very low: aflatoxins, 0.002–0.7 μg/kg; OTA, 0.07–0.25 μg/kg; ZEA, 1–3 μg/kg. The limits of determination were: aflatoxins, 0.25 μg/kg; OTA, 0.5 μg/kg; ZEA, 5 μg/kg. The recovery rates for aflatoxins, OTA, and ZEA for rye and rice were between 86 and 93% when a 0.5 g sample matter per immunoaffinity column was used.


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