Liquid Chromatographic Determination of Spiramycin Residues in Chicken Tissues

1986 ◽  
Vol 69 (4) ◽  
pp. 644-646
Author(s):  
Tomoko Nagata ◽  
Masanobu Saeki

Abstract A liquid chromatographic (LC) method is described for determination of spiramycin residues in chicken muscles. The drug is extracted from muscles with acetonitrile, the extract is concentrated to 3-4 mL and rinsed with n-hexane followed by ethyl ether, and the drug is extracted with chloroform. LC analysis is carried out on a Zorbax BP-C8 column, and spiramycin is detected spectrophotometrically at 231 nm. Recoveries of spiramycin added to chicken muscles at 0.2 and 0.1 ppm were 93.9 and 89.0%, respectively. The detection limit was 5 ng for spiramycin standard, and 0.05 ppm in chicken muscles.

1977 ◽  
Vol 60 (5) ◽  
pp. 1081-1086
Author(s):  
Oscar W Van Auken ◽  
Michael Hulse

Abstract Conditions are described for extraction, cleanup, derivatization, detection, and quantitation of hexachlorophene (HCP) residues from several types of plant material. Wet plant tissue was homogenized and extracted with ethyl ether, dried, and methylated with excess diazomethane. Samples were precleaned by column chromatography on silica gel with benzene-petroleum ether (1 + 1), and then 1–10 μI concentrated sample was chromatographed on a 6′ column of 3% SE-30 on 80–100 mesh Gas-Chrom Q. The detection limit for the electron capture detector was <0.1 ng dimethoxyhexachlorophene and 1 ppb HCP in plant tissue. Recoveries (%) of 11–610 pph HCP added to tissue averaged 94.3 for tomatoes, 86.4 for green peppers, 92.6 for cucumbers, 93.3 for green beans, 93.7 for peanut hay, and 91.6 for peanut shells.


1987 ◽  
Vol 70 (6) ◽  
pp. 1031-1032
Author(s):  
Yuuko S Endoh ◽  
Ryozo Yamaoka ◽  
Nobuo Sasaki

Abstract A liquid chromatographic (LC) method is described for the quantitative determination of sulfamoyldapsone (2-sulfamoyl-4,4'-diaminodiphenyl sulfone) in swine muscle, liver, kidney, and fat. Sulfamoyldapsone was extracted from tissues with acetonitrile saturated with n-hexane. The extract was washed with n-hexane saturated with acetonitrile, concentrated, and cleaned up by alumina column chromatography. Sulfamoyldapsone was separated on an ODS column by using acetonitrile-methanol-water (6 + 18 + 76) and was detected at 292 nm. Overall average recovery of sulfamoyldapsone added to tissues at levels of 0.1 and 0.5 /μg/g was 93.3% ± 6.0. Detection limit was 0.02 μg/g in these tissues.


1980 ◽  
Vol 63 (6) ◽  
pp. 1211-1214
Author(s):  
Etsuko Suzuki ◽  
Mihoko Matsuda ◽  
Atsushi Momose ◽  
Masaya Namekata

Abstract A sensitive and specific gas-liquid chromatographic (GLC) method has been developed for determining low levels of clopidol in chicken tissues. Clopidol is extracted from the tissues with methanol, and cleaned up on an alumina column and an anion exchange resin column with 0.1% acetic acid–methanol as eluate. Clopidol is methylated with diazomethane, and then determined by GLC. 2,4-Dinitro-l-chlorobenzene is used as an internal standard. The method is applicable to levels as low as 2 ppb in chicken tissues. Recoveries of 2–20 ppb clopidol added to tissues averaged 87% for muscle, 84% for liver, 80% for kidney, and 76% for fat.


1986 ◽  
Vol 69 (5) ◽  
pp. 856-859 ◽  
Author(s):  
Sheldon D West ◽  
Edgar W Day

Abstract A residue method is described for determination of the aquatic herbicide fluridone (1-methy1-3-phenyl-5-[3-(trifluoromethyl)phenyl]-4(1H)- pyridinone) and its metabolite (1-methy1-3-(4-hydroxyphenyl)-5-[3- (trifluoromethyl)phenyl]-4(1H)-pyridinone) in fish and crayfish tissues. Both compounds are extracted from tissues with methanol, and the extracts are subjected to acidic hydrolysis to release conjugated forms of fluridone and the metabolite. Sample extracts are purified by liquidliquid partitioning and Florisil Sep-Pak® column chromatography. Both compounds are separated and measured by reverse phase liquid chromatography with UV detection at 313 nm. In the absence of interfering peaks, the method has a detection limit of approximately 0.04 ppm of either compound. Overall, recoveries averaged 96% for fluridone and 78% for the metabolite for all tissue types combined.


1995 ◽  
Vol 78 (3) ◽  
pp. 841-845 ◽  
Author(s):  
Bertil Lindgren ◽  
Tomas Berglöf ◽  
Åsa Ramberg ◽  
Anna Stepdmska ◽  
Malin Åkerblom

Abstract A method is presented for rapid determination of bromide ion in commodities and blood by paired-ion liquid chromatography with electrochemical detection. The method involves extraction of samples with water and filtration. Blood is passed through a Sep-Pak C18 minicolumn. Recoveries are usually close to 100%, with satisfactory precision. The detection limit is 1 mg/kg. The method needs little labor and uses no noxious solvents or reagents.


1979 ◽  
Vol 62 (5) ◽  
pp. 1141-1145
Author(s):  
Charles W Luhning ◽  
Paul D Harman ◽  
Joe B Sills ◽  
Verdel K Dawson ◽  
John L Allen

Abstract A gas-liquid chromatographic (GLC) method is described for determining residues of Bayer 73 (2-aminoethanol salt of 2’,5-dichloro-4’-nitrosalicylanilide) in fish muscle, aquatic invertebrates, mud, and water by analyzing for 2-chloro-4-nitroaniline (CNA), a hydrolysis product of Bayer 73. Bayer 73 residues are extracted from fish muscle tissue, invertebrates, and mud with acetone-formic acid (98+2), and partitioned from water samples with chloroform. After sample cleanup by solvent and acid-base partitioning, the concentrated extract is hydrolyzed with 2N NaOH and H2O2 for 10 min at 95°C. The CNA is then partitioned into hexane-ethyl ether (7+3) and determined by electron capture GLC. Average recoveries were 88% for fish, 82% for invertebrates, 82% for mud, and 98% for water at 3 or more fortification levels.


1986 ◽  
Vol 69 (1) ◽  
pp. 70-71 ◽  
Author(s):  
Owen W Parks ◽  
Robert C Doerr

Abstract A procedure is described for the quantitation of Zoalene (3,5-dinitro-o-toluamide) and its 2 major monoamino metabolites in chicken tissues. The method includes blender extraction of tissue with chloroformethyl acetate (1 + 1), adsorption of the drug and metabolites on neutral alumina, and subsequent elution of the residues with pH 3.5 formate buffer-methanol (6.5 + 3.5). Recovered residues were separated on a 5 μ C18 column with the alumina eluting solvent as the LC mobile phase. The parent drug and metabolites were detected and quantitated with an electrochemical detector in the reductive mode with a minimum level of reliable measurement of 0.1 ppm. Overall mean recoveries greater than 85% were obtained with Zoalene and its 2 monoamino metabolites in breast, thigh, and liver tissues fortified with 0.25-2.00 ppm. The results on tissues from chickens fed a diet containing 0.0125% Zoalene are presented.


1986 ◽  
Vol 69 (6) ◽  
pp. 941-943
Author(s):  
Tomoko Nagata ◽  
Masanobu Saeki

Abstract A method is presented for determination of amprolium residues in chicken muscles by a liquid chromatographic post-column reaction system. The drug is extracted from muscles with methanol, and the extract is concentrated to 3-4 mL. This aqueous solution is rinsed with n-hexane and cleaned up by alumina column chromatography. The drug is separated from the interferences on a LiChrosorb RP-8 column, reacted with ferricyanide in alkaline solution, and quantitated by fluorometric detection at 367 nm (excitation) and 470 nm (emission). Recoveries of amprolium added to chicken muscles at levels of 0.1 and 0.2 ppm were 74.9 and 80.9%, respectively. The detection limit was 1 ng for amprolium standard and 0.01 ppm in chicken muscles.


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