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1.
A liquid chromatographic (LC) method is described for determination of olaquindox residues in swine tissues. The drug is extracted from tissues with acetonitrile, and the extract is evaporated to dryness. This residue is cleaned up by alumina column chromatography. LC analysis is carried out on a Nucleosil C18 column, and olaquindox is quantitated by ultraviolet detection at 350 nm. The average recoveries of olaquindox added to tissues at levels of 0.2, 0.1, and 0.05 ppm were 74.0, 68.6, and 66.3%, respectively. The detection limit was 2 ng for olaquindox standard and 0.02 ppm in tissues.  相似文献   

2.
Crossbred pigs weighing 80-110 kg were injected intramuscularly in the ham with 8.8 mg/kg tylosin. Animals were slaughtered in groups of 3 at intervals of 4 h, and 1, 2, 4, and 8 days after injection, and samples of blood, injected muscle, uninjected muscle, liver, and kidney were analyzed by liquid chromatography (LC) and by bioassay using Sarcina lutea as the test organism. The LC method was far more sensitive with a detection limit of less than 0.1 ppm, while the detection limit by bioassay was about 0.5 ppm in tissue. Results by bioassay and LC sometimes differed considerably for tissue samples. Residues in all tissues were below the tolerance limit of 0.2 ppm at 24 h, except in the injected muscle in one animal. Residues were not detected in any tissue of any animal at 48 h after treatment.  相似文献   

3.
A liquid chromatographic (LC) method is described for determination of ethopabate residues in chicken tissues. The drug is extracted from tissues with acetonitrile, and the extract is concentrated to 2-3 mL. This aqueous solution is rinsed with ethyl acetate and cleaned up by Florisil column chromatography. LC analysis is carried out on a Zorbax ODS column, and ethopabate is quantitated by using a fluorometric detector set at 306 nm (excitation) and 350 nm (emission). Recoveries of ethopabate added to chicken tissues at levels of 0.01 and 0.05 ppm were 87.8 and 92.7%, respectively. The detection limit was 100 pg for ethopabate standard, and 0.5 ppb in chicken tissues.  相似文献   

4.
An accurate, sensitive method is described for the determination of monensin residue in chicken tissues by liquid chromatography (LC), in which monensin is derivatized with a fluorescent labeling reagent, 9-anthryldiazomethane (ADAM), to enable fluorometric detection. Samples are extracted with methanol-water (8 + 2), the extract is partitioned between CHCl3 and water, and the CHCl3 layer is cleaned up by silica gel column chromatography. Free monensin, obtained by treatment with phosphate buffer solution (pH 3) at 0 degrees C, is derivatized with ADAM and passed through a disposable silica cartridge. Monensin-ADAM is identified and quantitated by normal phase LC using fluorometric detection. The detection limit is 1 ppb in chicken tissues. Recoveries were 77.6 +/- 1.8% at 1 ppm, 56.7 +/- 7.1% at 100 ppb, and 46.5 +/- 3.7% at 10 ppb fortification levels in chicken. Gas chromatography-mass spectrometry is capable of confirming monensin methyl ester tris trimethylsilyl ether in samples containing residues greater than 5 ppm.  相似文献   

5.
A liquid chromatographic (LC) method is described for the determination of neomycin in animal tissues. Tissues are homogenized in 0.2M potassium phosphate buffer (pH 8.0); the homogenate is centrifuged, and the supernate is heated to precipitate the protein. The heat-deproteinated extract is acidified to pH 3.5-4 and directly analyzed by LC. The LC method consists of an ion-pairing mobile phase, a reverse phase ODS column, post-column derivatization with o-phthalaldehyde reagent, and fluorometric detection. The LC method uses paromomycin as an internal standard, and separates neomycin from streptomycin or dihydrostreptomycin because they have different retention times. The LC column separates neomycin in 25 min; the detection limit is about 3.5 ng neomycin. The overall recovery of neomycin from kidney tissues spiked at 1-30 ppm was 96% with a 9.0% coefficient of variation. The method was also applied to muscle tissue.  相似文献   

6.
Tylosin, an antibiotic developed specifically for agricultural use, and erythromycin are the main macrolide antibiotics used in animal production. Two-dimensional thin layer chromatography has been used for detection of tylosin in poultry meat, eggs, and milk and for erythromycin in poultry meat. Detection limits reported are, for tylosin, 0.1 ppm in poultry meat, 0.05 ppm in egg, and 0.01 ppm in milk, and for erythromycin, 0.25 ppm in poultry meat. Liquid chromatography (LC) has also been used for determination of tylosin in milk, blood, and tissues of animals. Samples (milk, blood serum, or tissue homogenates in water or pH 2.2 buffer) were deproteinized with acetonitrile, tylosin was partitioned into methylene chloride, and the extracts were concentrated and dissolved in acetonitrile. Chromatography was done on a reverse phase end-capped C18 column using 0.002-0.005 M ammonium dihydrogen phosphate-acetonitrile-methanol (10 + 60 + 30-5 + 80 + 15). Solvent composition was varied with the type of sample analyzed. The method will detect 0.1 ppm tylosin in tissues and less in milk and blood serum. The LC method was more sensitive than microbiological assays for detection of tylosin in tissues of treated swine; recoveries of tylosin by the LC method were frequently several-fold higher.  相似文献   

7.
A liquid chromatographic (LC) method was developed to determine sedecamycin, a 17-membered macrolide antibiotic used for treating swine dysentery, and its major metabolites (lankacidin C, lankacidinol A, and lankacidinol) in swine plasma and tissues. Plasma is directly extracted with ethyl acetate and analyzed by liquid chromatography without purification. Tissues are homogenized in a phosphate buffer containing sodium chloride, and then extracted with ethyl acetate. The extracts are subjected to silica gel-Florisil, double-layered column chromatography to remove endogenous interfering substances. The LC determination uses silica gel and ODS-silica as a stationary phase. The detection limits for sedecamycin and its metabolites were less than or equal to 0.05 ppm, and average recoveries and coefficients of variation (0.2-1 ppm range) were greater than 75% and less than 10%, respectively.  相似文献   

8.
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.  相似文献   

9.
A sensitive, selective analytical method has been developed for determination of phenol in honey by liquid chromotography (LC) with amperometric detection (AMD). Phenol is extracted with benzene from the distillate of honey. The benzene extract is washed with 1% sodium bicarbonate solution and then reextracted with 0.1N sodium hydroxide followed by cleanup on a C18 cartridge. Phenol is determined by reverse-phase LC with amperometric detection. An Inertsil ODS column (150 X 4.6 mm, 5 microns) is used in the determination. The mobile phase is a mixture (20 + 80 v/v) of acetonitrile and 0.01M sodium dihydrogen phosphate containing 2mM ethylenediaminetetraacetic acid, disodium salt (EDTA) with the pH adjusted to 5.0. The flow rate is 1 mL/min under ambient conditions. The applied potential of the AMD using a glassy carbon electrode is 0.7 V vs an Ag/AgCl reference electrode. Average recoveries of phenol added to honey were 79.8% at 0.01 ppm spiking level, 90.4% at 0.1 ppm, and 91.0% at 1.0 ppm. Repeatabilities were 3.4, 1.3, and 1.8%, respectively. The detection limit of phenol in honey was 0.002 ppm. For analysis of 112 commercial honey samples, the range and average values of 32 detected samples were 0.05-5.88 ppm and 0.71 ppm, respectively.  相似文献   

10.
A liquid chromatographic (LC) method with fluorometric detection was developed to quantitatively determine residue levels of monensin, salinomycin, narasin, and lasalocid in beef liver tissue. The ionophores are extracted from the tissue, purified by both alumina and Sephadex LH-20 column chromatography, and then derivatized. Lasalocid was directly esterified with 9-anthryldiazomethane (ADAM), but monensin, salinomycin, and narasin were first acetylated with acetic anhydride and then esterified with ADAM. The ADAM derivatives were purified on a silica gel column and separated by LC using an RP C-8 5 micron column. A fluorescence detector set at 365 nm (excitation) and 418 nm (emission) was used to monitor the column effluent. The detection limits were 0.15 ppm, and the calibration curves were linear between 0.5 and 5.0 ppm for all 4 ionophores. Mean recoveries were 57, 70, 75, and 90% for lasalocid (5 ppm), monensin (2.5 ppm), salinomycin (2.5 ppm), and narasin (2.5 ppm), respectively. The ionophores were also separated and semiquantitated by using bioautography and thin layer chromatography with a vanillin spray.  相似文献   

11.
A new liquid chromatographic method for determination of ampicillin in canine and equine serum has been developed. The serum sample (500 microL) is vortex-mixed with 20% ethanol (500 microL) and filtered using a 30,000 molecular weight cutoff microseparation tube to separate high molecular weight solutes following low-speed centrifugation. Ampicillin is then separated from other serum components by reverse phase ion-pair liquid chromatography (LC). The ultraviolet (UV) absorbance of the column effluent is monitored at 230 nm. Recoveries of ampicillin from canine serum spiked at concentrations of 10, 40, and 60 micrograms/mL were 93.1, 100.9, and 87.8%, respectively, with coefficients of variation (CVs) of 2.91, 3.08, and 4.08%, respectively. Recoveries of ampicillin from equine serum spiked at the same concentrations were 91.6, 90.1, and 88.7%, respectively, with CVs of 3.03, 2.61, and 3.35%, respectively. The limit of detection for ampicillin by this method is less than 0.5 micrograms/mL serum.  相似文献   

12.
Sulfonamides are widely used as a feed additive in animal production in Japan. The present paper is a determination of 3 sulfonamides: sulfamethazine (SMZ), sulfamonomethoxine [SMX, 4-amino-N-(3-methoxypyrazinyl)-benzenesulfonamide], and sulfadimethoxine (SDX) in animal tissue and egg by liquid chromatography (LC). Tissues were extracted with acetonitrile and fat was removed by liquid/liquid partition. The sulfonamides were purified by an ODS cartridge column; then each compound was separated by an ODS LC column and detected at 268 nm. Quantification levels were 0.02 ppm for SMZ and SMX, and 0.04 ppm for SDX; detection limits were 0.01 ppm for SMZ and SMX, and 0.02 ppm for SDX. Calibration curves were linear between 2 and 40 ng for SMZ and SMX, and between 4 and 80 ng for SDX. Recoveries from muscle and egg samples spiked with 1-2 micrograms/10 g were 81-98%.  相似文献   

13.
Oxyfluorfen and oxyfluorfen amine were determined by liquid chromatography (LC) with ultraviolet (UV) and photoconductivity detection (PCD). A simple extraction procedure acceptably recovered both analytes from garbanzo beans over a wide range of fortifications (0.05 to 20 ppm) (83 +/- 4 for oxyfluorfen; 85 +/- 4 for oxyfluorfen amine). Percent recoveries decreased slightly as the fortification level decreased. Both analytes could be determined simultaneously at a concentration greater than 0.2 ppm in garbanzo beans. Detection limits were 3 ng for oxyfluorfen and 100 ng for oxyfluorfen amine using LC/UV, and 12 ng for both oxyfluorfen and oxyfluorfen amine with LC/PCD. Different knitted reaction coils and photoreactors were evaluated. Photoproduct yields and identification were determined by ion chromatography. The LC/PCD method measures oxyfluorfen and oxyfluorfen amine separately and has a shorter analysis time, while the standard method using gas chromatography measures total residues and is more sensitive.  相似文献   

14.
A rapid, sensitive, liquid chromatographic (LC) method has been developed for determination of residuals of the processing aid, 4-hexylresorcinol, on shrimp meat. An aqueous homogenate of shrimp meat is extracted with ethyl acetate followed by precolumn preparation on a silica Sep-Pak cartridge. LC determination is preformed with a Nova-Pak C18 column, with UV detection at 214 nm. Sensitivity was 0.006 micrograms, and recovery from shrimp meat samples of known 4-hexylresorcinol addition was 94%. Shrimp treated with 4-hexylresorcinol under the recommended dip protocol had mean residuals of 1.18 ppm, with a standard deviation of 0.13 ppm.  相似文献   

15.
A simple specific and rapid confirmatory method for determining the two amphoteric penicillins, that is, amoxicillin and ampicillin, in bovine muscle, liver, kidney, and milk is presented. This method is based on the matrix solid-phase dispersion technique with hot water as extractant followed by liquid chromatography (LC)-tandem mass spectrometry. With this instrumentation, the selected reaction monitoring acquisition mode with two fragmentation reactions for each analyte was adopted. After acidification and filtration of the aqueous extracts, 25 microL of the tissue final extracts and 50 microL of the milk final extract were injected into the LC apparatus. Absolute recovery of the two analytes in any biological matrix at the 50 ppb level in tissues and the 4 ppb level in milk was 74-95% with relative standard deviations (RSDs) of no larger than 9%. When penicillin V was used as surrogate internal standard, relative recovery of the targeted compounds present in bovine tissues and milk at, respectively, 25 and 2 ppb levels ranged between 100 and 106% with RSDs of no larger than 11%. When fractionation of analytes by using a short chromatographic run was attempted, remarkable signal weakening for the two analytes was experienced. This effect was traced to polar endogenous coextractives eluted in the first part of the chromatographic run that interfered with the gas-phase ion formation of the two penicillins. Slowing the chromatographic run eliminated this unwelcome effect. Limits of quantification of the two analytes in bovine milk were estimated to be <1 ppb, whereas amoxicillin and ampicillin could be quantified in bovine tissues down to 3.1 and 0.8 ppb levels, respectively.  相似文献   

16.
A simple method is presented for determination of menadione in vitamin premixes and feedstuffs by normal-phase liquid chromatography (LC). Vitamin K3 is extracted and converted to free menadione, which can be determined directly by LC analysis. Peak area or height is measured at 251 nm, and menadione is quantitated by comparison with the working standard. Menadione can be estimated with a detection limit of 2.5 ppm. Recoveries for premixes ranged from 97.3 to 98.3% and for feedstuffs from 93.7 to 96.8%. The method allows the assay of all commercial K3 compounds in pure or stabilized form and is applicable to a wide variety of feeds and premixes.  相似文献   

17.
A liquid chromatographic method is described for the quantitative measurement of nicarbazin in chicken liver, fat, muscle, and skin tissues. The 4,4'-dinitrocarbanilide (DNC) portion of nicarbazin is extracted from tissues with ethyl acetate. After filtration and evaporation, the extract is purified by liquid-liquid partitioning with acetonitrile-hexane and alumina cartridge chromatography. DNC is separated and measured by reverse-phase liquid chromatography (RP-LC) with an octadecylsilyl (ODS) column and a UV detector set at 340 nm. The overall average recovery of DNC added to tissues was 83.4 +/- 3.1%. The lowest level validated in tissues by this procedure was 0.10 ppm. The limit of detection was estimated to be 0.020 ppm. This method provides a sensitive, selective, rapid, and reproducible alternative to existing purification, separation, and detection techniques, such as differential pulse polarography and colorimetry, for determination of nicarbazin in chicken tissues. Identity of DNC is confirmed by subjecting the purified extracts to thermospray-LC/mass spectrometric analysis using negative-ion detection and selected ion monitoring. Three structural-indicating ions at m/z 302, 272, and 164 are monitored in the thermospray-mass spectrum which are characteristic of the DNC molecule.  相似文献   

18.
A liquid chromatography (LC) method for determining the hypoxanthine content in fish tissues has been developed. Hypoxanthine is extracted with 0.6M perchloric acid, and determined by LC on a reverse phase microparticulate column with UV absorbance detection. The mobile phase is 0.01M potassium phosphate buffer (pH 4.5). The percent relative standard deviation for measurements by the recommended method was less than 7% with a detection limit of 10 ng. Recoveries of hypoxanthine added to various fish tissues were better than 90%. The operational errors, interferences, and recoveries for spiked samples have been investigated and compare favorably with an established xanthine oxidase enzyme method. The described LC method is simple, rapid, and specific for measuring hypoxanthine content in various fish tissues. Some post-mortem studies have indicated the method may also be used for the determination of adenosine monophosphate, inosine monophosphate, and inosine.  相似文献   

19.
The Onley-Yip procedure for determining ethylenethiourea (ETU) in milk and crops was modified to reduce interferences by the ethylenebisdithiocarbamates (EBDCs). A 20 g crop-methanol extract is cleaned up by adsorbing the sample onto Gas-Chrom S. desorbing ETU, and eluting ETU from aluminum oxide with chloroform containing ethanol. ETU is converted to the S-butyl derivative for gas-liquid chromatography (GLC) and flame photometric detection (sulfur mode). For liquid chromatography (LC), ETU is cleaned up on another aluminum oxide column and injected directly. LC and GLC results are confirmed by thin layer chromatography. A cooking procedure based on conversion of EBDCs to ETU is included for surveying crops for possible EBDC content. Recoveries from 8 crops and milk fortified at 0.05 ppm ETU ranged from 73 to 100%.  相似文献   

20.
Residue methodology is described for the determination of AC 217,300 residues in pasture grass and crop samples. After extraction and subsequent cleanup on an XAD-2 column, residues of AC 217,300 are determined by liquid chromatography (LC), using a reverse phase paired-ion chromatographic system and detection at 300 nm. The method has a validated limit of sensitivity of 0.05 ppm with corresponding control values for the commodities analyzed of less than 0.01 ppm. Apparent residues over 0.05 ppm can be confirmed by either gas chromatography with an electron capture detector (GC-EC) or gas chromatography-negative ion chemical ionization mass spectrometry (GC-NICI). The direct GC-NICI method circumvents the need for sample cleanup on the XAD-2 column, and offers a greatly simplified procedure that is useful for screening samples. Recoveries of AC 217,300 from the commodities analyzed have been satisfactory with all methods of analysis.  相似文献   

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