scholarly journals Determination of Residues of Flumequine and 7-Hydroxyflumequine in Edible Sheep Tissues by Liquid Chromatography with Fluorimetric and Ultraviolet Detection

1998 ◽  
Vol 81 (3) ◽  
pp. 519-527 ◽  
Author(s):  
Jean-michel Delmas ◽  
Anne-marie Chape ◽  
Pascal Sanders
Keyword(s):  
Liquid Chromatography ◽  
Ethyl Acetate ◽  
Simultaneous Determination ◽  
Rapid Method ◽  
Active Metabolite ◽  
Fluorimetric Detection ◽  
Ultraviolet Detection ◽  
Tissue Extracts ◽  
Edible Tissues

abstract A simple, sensitive, and rapid method for simultaneous determination of residues of flumequine and its microbiologically active metabolite 7-hydroxyflumequine in 100 mg sheep edible tissues (muscle, liver, kidney, and fat) by liquid chromatography is reported. After liquid-liquid cleanup with ethyl acetate, tissue extracts were injected onto a Select B column. The 2 compounds were determined by ultraviolet and fluorimetric detection. The method was repeatable and reproducible for flumequine and 7-hydroxyflumequine in muscle, liver, kidney, and fat, with limits of detection below 2 and 3 μg/kg for flumequine and 7-hydroxyflumequine, respectively. Mean recoveries for flumequine were 90 ± 7, 82 ± 7,89 ± 5, and 82 ± 6% in muscle, liver, kidney, and fat, respectively. Mean recoveries for 7-hydroxyflumequine were 91 ± 2, 90 ± 4, 86 ± 3, and 84 ± 4% in muscle, liver, kidney, and fat, respectively.

scholarly journals Simultaneous Determination of Residual Antiparasitic Lactones in Bovine Muscle and Liver by Liquid Chromatography with Fluorescence Detection

2003 ◽  
Vol 86 (3) ◽  
pp. 490-493 ◽  
Author(s):  
Tomoko Nagata ◽  
Fumio Miyamoto ◽  
Yasuyuki Hasegawa ◽  
Eiichi Ashizawa
Keyword(s):  
Liquid Chromatography ◽  
Ethyl Acetate ◽  
Simultaneous Determination ◽  
Fluorescence Detection ◽  
Dimethyl Formamide ◽  
Bovine Muscle

Abstract Abamectin, doramectin, eprinomectin, ivermectin, milbemectin, and moxidectin in bovine muscle and liver were extracted with acetonitrile. The extracts were partitioned with n-hexane and then evaporated to dryness. The residue was cleaned up on Bond Elute NH2 cartridge, and the drugs were eluted from the cartridge with methanol–ethyl acetate (3 + 7). The eluate was evaporated to dryness, and residues were derivatized with N,N-dimethyl-formamide–acetic anhyride-1-methylimidazole. The derivatives were determined by liquid chromatography with fluorescence detection. Recoveries of the 6 drugs were 79.6–63.8% in muscle and 71.6–60.6% in liver at 0.01 ppm levels. The quantitation limits were 5 ppb for each drug.

Simultaneous determination of disopyramide and mono-N-dealkyldisopyramide enantiomers in plasma and urine by use of a chiral cellulose-derivative column

1990 ◽  
Vol 36 (7) ◽  
pp. 1300-1304 ◽  
Author(s):  
H Echizen ◽  
K Ochiai ◽  
Y Kato ◽  
K Chiba ◽  
T Ishizaki
Keyword(s):  
Simultaneous Determination ◽  
Active Metabolite ◽  
Signal To Noise Ratio ◽  
Plasma Concentrations ◽  
Internal Standard ◽  
Cellulose Derivative ◽  
Ultraviolet Detection ◽  
Lower Detection ◽  
Relative Errors

Abstract This assay allows simultaneous determination of the enantiomers of both disopyramide and its active metabolite, mono-N-dealkyldisopyramide, in 1 mL of plasma or 0.1 mL of urine within approximately 35 min by HPLC with a chiral cellulose-derivative column and ultraviolet detection. Recoveries for the analytes and the internal standard (racemic verapamil) with an extraction from alkalinized plasma or urine into diethyl ether were greater than 90%. Intra- and interassay CVs for disopyramide enantiomers were less than 5.5% at 2.5 mg/L in plasma and less than 6.5% at 25 mg/L in urine; for mono-N-dealkyldisopyramide enantiomers they were less than 6.3% and less than 8.9%, respectively. Intra- and interassay relative errors for determining these analytes in plasma and urine at 2.5 and 25 mg/L, respectively, ranged from -5.9% to +2.5%. The calibration curves for the respective analytes were linear (r = 0.995 or greater, P less than 0.01) from 0.025 to 5.0 mg/L in plasma and from 0.5 to 10 mg/L in urine. The lower detection limits (signal-to-noise ratio of 3) for S(+)-disopyramide and the other analytes were 0.010 and 0.025 mg/L, respectively. We evaluated clinical applicability of this method by determining steady-state plasma concentrations and urinary excretions of the respective analytes in a pediatric patient being treated with racemic disopyramide.

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