scholarly journals Liquid Chromatographic Determination of Acriflavine and Proflavine Residues in Channel Catfish Muscle

1997 ◽  
Vol 80 (3) ◽  
pp. 486-490
Author(s):  
Steven M Plakas ◽  
Kathleen R El Said ◽  
Edward L E Jester ◽  
F Aladar Bencsath ◽  
William L Hayton

Abstract A liquid chromatographic (LC) method was developed for determination of acriflavine (ACR) and proflavine (PRO) residues in channel catfish muscle. Residues were extracted with acidified methanol solution, and extracts were cleaned up with Ci& solid-phase extraction columns. Residue concentrations were determined on an LC cyano column, with spectrophotometric detection at 454 nm. Catfish muscle was individually fortified with ACR (purified from commercial product) and PRO at concentrations of 5,10,20, 40, and 80 ppb (5 replicates per level). Mean recoveries from fortified muscle at each level ranged from 86 to 95%, with relative standard deviations (RSDs) of 2.5 to 5.7%. The method was applied to incurred residues of ACR and PRO in muscle after waterborne exposure of channel catfish to commercial acriflavine (10 ppm total dye for 4 h). RSDs for incurred residues of ACR and PRO were in the same range as those for fortified muscle. Low residue concentrations (<1 % of exposure water concentration) suggested poor absorption of ACR and PRO in catfish.

1994 ◽  
Vol 77 (4) ◽  
pp. 871-875 ◽  
Author(s):  
Jeffery R Meinertz ◽  
Verdel K Dawson ◽  
William H Gingerich ◽  
Bea Cheng ◽  
Mark M Tubergen

Abstract A liquid chromatographic method is described for the determination of sarafloxacin hydrochloride residues in channel catfish (Ictalurus punctatus) fillets. Sarafloxacin was extracted from fillet tissue with acetonitrile–water (1+1). The extract was centrifuged and the supernatant was partitioned with hexane. The aqueous fraction was filtered through a 0.45 μm filter and evaporated to dryness. The sample was redissolved with 20% acetonitrile–methanol (3 + 2) and 80% trifluoroacetic acid (0.1%), centrifuged, and filtered to remove proteins. Samples were analyzed by chromatography with gradient elution on a C18 column and with fluorescence detection (excitation at 280 nm and emission above 389 nm). Mean recoveries ranged from 85.4 to 104%, and relative standard deviations ranged from 1.06 to 5.58% in samples spiked at concentrations of 10.0–863.8 ng/g. The method detection limit for sarafloxacin was 1.4 ng/g.


1993 ◽  
Vol 76 (3) ◽  
pp. 531-534 ◽  
Author(s):  
Robert P Snell

Abstract A liquid chromatographic procedure is described for the determination of phthalide, monobutyl phthalate, and mono-2-ethylhexyl phthalate leached by water from solution administration sets. Recoveries varied from 88.8% for phthalide at 1 (μg/50 mL to 113% for monobutyl phthalate at 6 μg/50 mL. Relative standard deviations at 1 μg/50 mL were 2.59% for phthalide, 3.54% for monobutyl phthalate, and 11.6% for mono-2- ethylhexyl phthalate. At 6 μg/50 mL, the relative standard deviation for mono-2-ethylhexyl phthalate decreased to 3.88%. Reproducibilities for 5 standard injections were 1.40% for phthalide, 1.84% for monobutyl phthalate, and 1.95% for mono-2- ethylhexyl phthalate. Correlation coefficients were 1.00 for the 3 compounds. Five sets from 2 manufacturers were examined. No phthalide or monobutyl phthalate was found. One manufacturer’s sets contained 37.6-44.4 μg/L mono-2- ethylhexyl phthalate. The sample matrix had some interference if phthalide or monobutyl phthalate was present.


1998 ◽  
Vol 81 (4) ◽  
pp. 702-708 ◽  
Author(s):  
Jeffery R Meinertz ◽  
Guy R Stehly ◽  
William H Gingerich

Abstract The approved use of oxytetracycline (OTC) in U.S. aquaculture is limited to specific diseases in salmonids and channel catfish. OTC may also be effective in controlling diseases in other fish species important to public aquaculture, but before approved use of OTC can be augmented, an analytical method for determining OTC in fillet tissue from multiple species of fish will be required to support residue depletion studies. The objective of this study was to develop and validate a liquid chromatographic (LC) method that is accurate, precise, and sensitive for OTC in edible fillets from multiple species of fish. Homogenized fillet tissues from walleye, Atlantic salmon, striped bass, white sturgeon, rainbow trout, and channel catfish were fortified with OTC at nominal concentrations of 10, 20, 100,1000, and 5000 ng/g. In tissues fortified with OTC at 100,1000, and 5000 ng/g, mean recoveries ranged from 83 to 90%, and relative standard deviations (RSDs) ranged from 0.9 to 5.8%. In all other tissues, mean recoveries ranged from 59 to 98%, and RSDs ranged from 3.3 to 20%. Method quantitation limits ranged from 6 to 22 ng/g for the 6 species. The LC parameters produced easily in teg ratable OTC peaks without coelution of endogenous compounds. The method is accurate, precise, and sensitive for OTC in fillet tissue from 6 species of fish from 5 phylogenetically diverse groups.


2005 ◽  
Vol 88 (5) ◽  
pp. 1292-1298 ◽  
Author(s):  
Wendy C Andersen ◽  
José E Roybal ◽  
Sherri B Turnipseed

Abstract A liquid chromatography (LC) method is presented for the quantitative determination of malachite green (MG) in salmon. MG and leucomalachite green (LMG) residues were extracted from salmon tissue with ammonium acetate buffer and acetonitrile, and then isolated by partitioning into dichloromethane. LMG was quantitatively oxidized to the chromic MG by reaction with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone. Samples were then cleaned up by solid-phase extraction with alumina and propylsulfonic acid phases. Extracts were analyzed for MG by LC with visible detection at 618 nm using isocratic elution and a C18 column. The method was validated in 35 farm-raised salmon (Salmo salar) tissues fortified at 1, 2, 4, and 10 ng/g (ppb) with an average recovery of 95.4% and a relative standard deviation of ±11.1%, and in 5 canned salmon (Oncorhynchus gorbuscha) samples fortified at 10 ng/g with an average recovery of 88.9 ± 2.6%. This study also included the determination of MG and LMG residues in tissues from salmon that had been treated with MG. MG was quantitatively determined at the method detection limit of 1 ng/g.


2003 ◽  
Vol 68 (11) ◽  
pp. 883-892 ◽  
Author(s):  
Dragica Zendelovska ◽  
Trajce Stafilov

A rapid, specific and sensitive high-performance liquid chromatographic method for the determination of famotidine in human plasma has been developed. Famotidine and the internal standard were chromatographically separated from plasma components using a Lichrocart Lichrospher 60 RP select B cartridge for solid-phase separation with a mobile phase composed of 0.1 % (v/v) triethylamine in water (pH 3) and acetonitrile (92:8, v/v). UV detection was set at 270 nm. The calibration curve was linear in the concentration range of 10.0 ? 350.0 ng mL-1. The method was implemented to monitor the famotidine levels in patient samples.


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