Automated gas chromatographic method for the determination of ethanol in canned salmon

A method has been developed for the determination of ethanol in canned salmon using automated headspace sampling in conjunction with analysis by gas chromatography. The thermal process for the commercial sterilization of canned salmon is shown to provide an effective extraction of the ethanol so that the fluid removed from the can may be used as the analytical sample with minimal preparation prior to analysis. Ethanol content is measured directly, without the need for an internal standard, by either GC/MS or GC/FID. The headspace autoanalyzer allows for a rapid determination of ethanol with greater reproducibility than could be obtained with manual injection systems. The GC/MS technique can also provide an advantage in that simultaneous single ion monitoring of the two major ethanol ions provides additional protection from interferences. To assess the applicability of this technique to other substrates, Atlantic sea scallop meats were also successfully analyzed by this technique.     

Fluorescence of muscle and connective tissue from cod and salmon

Autofluorescence of salmon and cod muscle was measured and compared with autofluorescence of collagen type I and type V. Similarities between fluorescence of fish muscle and collagen were found in that the same peaks were obtained around 390, 430, and 480 nm. These similarities are supported by principal component analyses. Texture and gaping score were predicted from the fluorescence spectra by partial least-squares regression. However, the predictions did not perform well. Relating fluorescence to the gaping score gave a prediction error of 0.91 and a correlation of 0.43 when measuring gaping on a scale from 0 to 5. There was no relation between texture and fluorescence spectra. Fluorescence of fish muscle could be related to the storage time. However, this relation seemed not to be induced by changes in collagen.     

Validation of an analytical methodology for determination of oxytetracycline and tetracycline residues in honey by HPLC with fluorescence detection

An analytical method for the determination of OTC and TC residues in honey was developed. Sample treatment involves an extraction in EDTA-McIlvaine buffer, followed by a solid-phase cleanup step. With regard to the cleanup procedure, different SPE cartridges were evaluated and the results presented. The method was validated according to the guidelines laid down by the 2002/657/EC European Decision parameters: decision limit (Cc alpha) and detection capability (CC beta) were 20 and 21 microg/Kg and 49 and 50 microg/Kg for OTC and TC, respectively, and recoveries of OTC and TC from spiked samples, at three fortification levels, were higher than 87% for both compounds. The analytical method was applied to 57 honey samples.     

A rapid method for nitrogen determination in plant tissue

Abstract

A method is described for determining the total N content of plant tissue by a modified Kjeldahl digestion employing a Technicon Auto‐Analyzer. It is faster than the manual AOAC Kjeldahl method. Reproducibility is not as good as that for the AOAC method, but coefficients of variability are comparable with those for the analyses of mineral elements in plant tissue by emission spectroscopy.     

Headspace gas chromatographic method for determination of ethanol in canned salmon: collaborative study

Six laboratories collaboratively studied a headspace gas chromatographic method for determination of ethanol in the aqueous phase of canned salmon. Ethanol is determined by a headspace sampling technique with tert-butanol as the internal standard, using a gas chromatograph equipped with a Super Q column and a flame ionization detector. With outliers excluded, the mean recoveries from samples spiked with 25.1 and 78.4 ppm ethanol were 112 and 110%, respectively. For the 4 sample pairs quantitated, repeatability coefficients of variation ranged from 1.42 to 4.25% and reproducibility coefficients of variation from 2.55 to 8.09%, with 3 of the 4 reported values less than 5%. The method has been adopted official first action.     

Capillary gas chromatographic method for determination of benzylpenicillin and other beta-lactam antibiotics in milk

A capillary gas chromatographic method is described for determining residues of beta-lactam antibiotic residues in milk, with specificity for benzylpenicillin (penicillin G), phenoxymethylpenicillin, methicillin, oxacillin, cloxacillin, dicloxacillin, and nafcillin. Residues are extracted from milk with acetonitrile. Samples are cleaned up by partitioning between aqueous and organic phases at different pH values. The penicillin residues are methylated with diazomethane to render them amenable to determination by gas chromatography on a methyl silicone fused silica column. Samples are introduced by split/splitless injection using a programmed temperature vaporization injector and are detected by nitrogen-selective thermionic detection. Internal standardization is used for quantitation. The limits of detection for all penicillins are well below 1 microgram/kg. Recoveries of spiked samples at 3 and 10 micrograms/kg are in the range of 42-85% (coefficients of variation 2-5%) and 41-92% (coefficients of variation 3-7%), respectively.     

Quantitative determination of nitrogen content in plant tissue by a colorimetric method

Abstract

This study was to evaluate the applicability of a colorimetric method in measuring the nitrogen (N) concentration in samples of vegetable origin. In order to do this, the same samples were analyzed with a colorimetric, and macro‐ and microKjeldahl methods. The colorimetric method has been used successfully in the determination of N in nutritional studies with rats and humans. The present procedure has the advantage of eliminating the distillation and titration steps of the Kjeldahl method and it is practical for nutritional studies, since many samples can be run in a single day. The N concentration was measured in leaves of two tropical grasses: Paspalum fasciculatum Willd. ex Flugge and Hyparrhenia rufa (Nees) Stapf, and a Standard Reference Material (SRM 1547 Peach Leaves). In all cases, there were no significant difference (P>0.05) in N concentration in these plant materials using the colorimetric, and micro‐ and macroKjeldahl methods. There was a good agreement between the N concentration of Peach leaves determined by the colorimetric method (2.94%) and the certified N concentration (2.94%). Hyparrhenia rufa, the African grass, and P. fasciculatum, the native species, showed very low N concentration in their leaves, respectively. These results indicate that the colorimetric method, with some light adjustments, is capable of determining the N concentration in plant samples of diverse origin and in very low N levels. The low N concentrations of the grass species suggest the strong limitation imposed by the low soil fertility for the growth and establishment of forage species in tropical savannas.     

Determination of oxolinic acid residues in salmon muscle tissue by liquid chromatography with fluorescence detection

The present paper describes a method for determination of oxolinic acid in salmon muscle tissue. Tissue (0.5-2 g) mixed with 2 g anhydrous sodium sulfate is extracted twice with ethyl acetate, centrifuged, and the extract evaporated. The residue is partitioned in a mixture of hexane and 0.01M oxalic acid and the aqueous phase chromatographed using fluorescence detection at 327 nm excitation and 369 nm emission. Calibration and standard curves are linear from 10-200 ppb and 100-2000 ppb at different sensitivity settings. Recoveries ranged from 71-83% in spiked blanks, with a CV of 4-10.3% over a 2-week period. Preliminary results in treated salmon were variable, possibly because some fish refused to eat medicated feed.     

A field method for the determination of total nitrogen in plant tissue

Abstract

While studying sward quality in Kenya, East Africa, we established a field laboratory for the determination of total nitrogen. Using Kjeldahl digestion procedures and an indophenol colorimetric method, we successfully analyzed over 900 plant and fecal samples while living in a tent camp. Variation from one digestion to the next was corrected for by using a grass standard with each digestion. Independent tests by other laboratories verified the accuracy of our methods.     

Colorimetric determination of tetracycline hydrochloride in pharmaceutical preparations

A simple, sensitive, and rapid colorimetric method is presented for the estimation of tetracycline hydrochloride as the pure drug and in formulations. The proposed method is based on the reaction of tetracycline HCl with cupric chloride in an alkaline medium to give a yellowish green solution whose absorbance is measured at 400 nm against a reagent blank. The color obeys Beer's law in the concentration range of 0-20 micrograms/mL. Molar absorptivity and Sandell's sensitivity of the yellowish-green copper complexes of tetracycline HCl are 1.99 X 10(4) L X mol-1 X cm-1 and 0.0241 ppm, respectively.     

Colorimetric determination of tetracycline derivatives in pharmaceutical preparations

A quick colorimetric method is reported for the determination of tetracycline derivatives such as oxytetracycline hydrochloride (OTCH), chlortetracycline hydrochloride (CTCH), methacycline hydrochloride (MCH), and doxycycline hydrochloride (DCH). The method involves complexation of the above derivatives with cupric chloride in alkaline medium. The yellowish green copper complexes of OTCH, CTCH, MCH, and DCH show maximum absorbance at 395, 410, 400, and 400 nm, respectively. The color intensity obeys Beer's law in the concentration range of 0-20 micrograms/mL.     

Improved HPLC method for determination of phytosiderophores in root washings and tissue extracts

Phytosiderophores (PS) of the mugineic acid family can be separated effectively by HPLC on resin‐based anion exchange columns. Using gradient elution with aqueous NaOH, separation of 2'‐deoxymugineic acid (DMA), mugineic acid (MA), 3‐hydroxymugineic acid (HMA), 3‐epi‐hyydroxymugineic acid (epi‐HMA), and nicotianamine was obtained within 16 min with a complete cycle time of 30 min. Fluorimetric detection was performed after post‐column derivatization using sodium hypochlorite (NaOCl) and orthophtaldialdehyde. External standardization revealed a linear range between 0.1–2.5 nmol of each compound applied to the column, with a detection limit of approximately 0.05 nmol. Only minimal sample pre‐treatment by addition of sodium hydroxide (NaOH) was required prior to HPLC‐injection of natural occurring samples such as root exudates, collected from the whole root system or from single apical root zones, xylem sap, and hot water extracts of root material, obtained from iron (Fe)‐deficient maize and barley plants. The method is discussed in comparison with cation exchange HPLC which is conventionally employed for the separation of phytosiderophores.     

A rapid confirmatory method for analyzing tetracycline antibiotics in bovine, swine, and poultry muscle tissues: matrix solid-phase dispersion with heated water as extractant followed by liquid chromatography-tandem mass spectrometry

A rapid, specific, and sensitive procedure for determining four widely used tetracycline antibiotics and three related epimers in bovine, swine, and poultry muscle tissues is presented. The method is based on the matrix solid-phase dispersion technique with heated water as the extractant followed by liquid chromatography (LC)-tandem mass spectrometry (MS) equipped with an electrospray ion source. Target compounds were extracted from tissues with 5 mL of water heated at 70 degrees C. After acidification and filtration, 100 microL of the aqueous extract was injected in the LC column. MS data acquisition was performed in the multireaction monitoring mode, selecting two precursor ion to product ion transitions for each target compound. Heated water appeared to be an excellent extractant, since the absolute recovery data ranged between 70 and 78%. The accuracy of the method was determined at three spike levels, using minocycline as a surrogate analyte, in any different kind of muscle tissues considered and varied between 88 and 109% with relative standard deviations ranging between 3 and 11%. Limits of quantification were estimated to range between 1 (chlortetracycline) and 9 ng/g (4-epioxytetracycline), based on a signal-to-noise ratio of 10, and are well below the tolerance levels set by the European Union. The effects of the extraction temperature, volume of the extractant, and washing of the material supporting the biological matrix with ethylenediamine tetraacetic disodium salt on the analyte recovery were studied.     

Liquid chromatographic determination of tetracycline residues in animal feeds

A liquid chromatographic method for the multiresidue determination of tetracyclines (TCs) in feeds is described. The levels of quantitation were 10 ppm each for tetracycline-HCl (TC), oxytetracycline (OTC), and chlortetracycline-HCl (CTC); the detection limit was 40 ppb for each. The calibration curves were linear between 2.5 and 100 ppm. The procedure involved double extraction with pH 2.0 and pH 4.5 McIlvain buffers, cleanup on a Sephadex LH-20 column, separation on a Nova-Pak C18 column, and detection at 370 nm. Recoveries of 10 micrograms/g of each TC in multiresidue feed samples ranged from 55.8 to 75.5% for OTC, 71.6 to 100% for TC, and 22.4 to 60.6% for CTC. The identities of the TCs were confirmed by thin layer chromatography.     

Boron determination in plant tissue by the azomethine H method

Abstract

A colorimetric method using the azomethine H reagent is described for determining boron in an acid extract of plant tissue ash. The method consistently gave the certified value of 33±3 ppm B for NBS orchard leaf reference material No. 1571 with 3.2% coefficient of variation. Samples were dry ashed and the ash extracted in 10 ml 0.36 N H₂SO₄ for 1 hr. at room temperature. Several acidic extractants and extracting conditions were compared which gave the certified value, but involved heating and readjusting the final volume.     

Matrix solid-phase dispersion extraction and gas chromatographic determination of chloramphenicol in muscle tissue

A method based on matrix solid-phase dispersion (MSPD) was developed for the gas chromatographic (GC) determination of chloramphenicol (CAP) residues in animal muscle tissue. Muscle tissue was blended with octadecylsilyl-derivatized silica (C(18)). A column made from the C(18)/muscle tissue matrix was washed with n-hexane and acetonitrile/water (5 + 95), after which CAP was eluted with acetonitrile/water (50 + 50) and partitioned into ethyl acetate. The final extract was evaporated, and a trimethylsilyl derivative of CAP was prepared with Sylon HTP and detected by GC with an electron capture detector (ECD) and a mass spectrometer. For quantitation, the internal standard used was the meta isomer of CAP (m-CAP) for GC-ECD. Muscle tissue samples were fortified at three concentration levels. At 5, 10, and 15 microg/kg levels the respective mean recoveries were 93, 96, and 98%, and the repeatabilities were 13, 11, and 3%. The detection and quantitation limits with ECD were 1.6 and 4.0 microg/kg, respectively. No statistically significant difference was observed in the efficiency of CAP extraction from muscle tissue of various animals (bovine, porcine, and poultry) by the MSPD technique.     

Determination of tetracycline antibiotics in beef and pork tissues using ion-paired liquid chromatography

A simplified procedure was developed for determination of tetracycline antibiotics in tissues which improved stability of these compounds in sample extracts and eliminated the need for troublesome cleanup procedures. Tissues were homogenized in water. Acetonitrile (16 mL) and then 1 mL of 0.1 M H(3)PO(4) were added to 4 mL of homogenate and the clear supernatant was filtered. The filtrate was mixed with hexane and dichloromethane and the resulting water layer was collected, evaporated to 1-2 mL, and filtered into autosampler vials. Ion-pairing liquid chromatography was used to separate tetracyclines from interferences in sample extracts, eliminating the need for further cleanup. Analysis was isocratic using a Phenomonex Prodigy ODS(3) column with a mobile phase of 4 mM oxalic acid, 4 mM sodium oxalate, 10 mM sodium decanesulfonate-acetonitrile (70 + 30 for oxytetracycline and tetracycline; 66 + 34 for chlortetracycline). Recoveries were generally in the 90-100% range with limits of quantitation of 0. 05-0.1 ppm. The procedure was evaluated with beef and pork muscle, liver, and kidney.     

光催化降解沼液中四环素类抗生素效果及反应动力学研究

该文采用光催化降解途径探究沼液中四环素类抗生素降解的最佳光源、pH值以及光催化对不同初始质量浓度抗生素的降解效果,同时进行不同初始浓度、pH值条件下抗生素光催化降解动力学研究。结果表明:不同光源对四环素类抗生素的降解效果为:高压汞灯紫外消毒灯长弧氙灯无光。高压汞灯催化2 h后,四环素、土霉素、金霉素的降解率分别达到91.68%、85.58%、81.18%。四环素类抗生素的初始质量浓度越低,光催化效果越好。四环素、土霉素、金霉素初始质量浓度为5 mg/L时,其降解率最高可达94.80%、88.35%和95.39%,沼液初始pH值对四环素、金霉素的降解率影响存在显著性差异(P0.05)。当pH值为6时,四环素的降解率最大为96.16%,反应速率常数为1.5971h-1,半衰期为0.355 3 h;当pH值为10时,金霉素的降解率最大为90.47%,反应速率常数为1.084 4 h-1,半衰期为0.338 3 h。沼液初始pH值对土霉素的降解率影响无显著差异(P0.05)。当pH值为10时,3种抗生素的平均降解率最大为89.88%。采用高压汞灯在沼液初始pH值为10时,催化降解5 mg/L四环素类抗生素效果最佳。