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Showing papers in "Journal of AOAC International in 2003"


Journal ArticleDOI
TL;DR: A simple, fast, and inexpensive method for the determination of pesticide residues in fruits and vegetables is introduced and effectively removes many polar matrix components, such as organic acids, certain polar pigments, and sugars, to some extent from the food extracts.
Abstract: A simple, fast, and inexpensive method for the determination of pesticide residues in fruits and vegetables is introduced. The procedure involves initial single-phase extraction of 10 g sample with 10 mL acetonitrile, followed by liquid-liquid partitioning formed by addition of 4 g anhydrous MgSO4 plus 1 g NaCl. Removal of residual water and cleanup are performed simultaneously by using a rapid procedure called dispersive solid-phase extraction (dispersive-SPE), in which 150 mg anhydrous MgSO4 and 25 mg primary secondary amine (PSA) sorbent are simply mixed with 1 mL acetonitrile extract. The dispersive-SPE with PSA effectively removes many polar matrix components, such as organic acids, certain polar pigments, and sugars, to some extent from the food extracts. Gas chromatography/mass spectrometry (GC/MS) is then used for quantitative and confirmatory analysis of GC-amenable pesticides. Recoveries between 85 and 101% (mostly > 95%) and repeatabilities typically < 5% have been achieved for a wide range of fortified pesticides, including very polar and basic compounds such as methamidophos, acephate, omethoate, imazalil, and thiabendazole. Using this method, a single chemist can prepare a batch of 6 previously chopped samples in < 30 min with approximately 1 dollar (U.S.) of materials per sample.

4,376 citations


Journal ArticleDOI
TL;DR: The proposed submersion method considerably decreases the extraction time required to complete a batch of samples, and the increase in throughput is very desirable in the quest for faster turnaround times and the greater efficiency in the use of labor.
Abstract: A method for determining crude fat in animal feed, cereal grain, and forage (plant tissue) was collaboratively studied Crude fat was extracted from the animal feed, cereal grain, or forage material with diethyl ether by the Randall method, also called the Soxtec method or the submersion method The proposed submersion method considerably decreases the extraction time required to complete a batch of samples The increase in throughput is very desirable in the quest for faster turnaround times and the greater efficiency in the use of labor In addition, this method provides for reclamation of the solvent as a step of the method The submersion method for fat extraction was previously studied for meat and meat products and was accepted as AOAC Official Method 99136 Fourteen blind samples were sent to 12 collaborators in the United States, Sweden, Canada, and Germany The within-laboratory relative standard deviation (repeatability) ranged from 109 to 926% for crude fat Among-laboratory (including within) relative standard deviation (reproducibility) ranged from 10 to 210% The method is recommended for Official First Action

227 citations


Journal ArticleDOI
TL;DR: A rapid, easy, and simple spectrophotometric method was developed for the estimation of total alkaloids precipitated by Dragendorff's reagent (DR) in plant materials based on the formation of yellow bismuth complex in nitric acid medium with thiourea.
Abstract: A rapid, easy, and simple spectrophotometric method was developed for the estimation of total alkaloids precipitated by Dragendorff's reagent (DR) in plant materials. It is based on the formation of yellow bismuth complex in nitric acid medium with thiourea. The yellow-colored complex formed obeys Lambert-Beer's law in the concentration range of 0.06-50 microg/mL with lambdamax at 435 nm. Using this method, the alkaloidal percentage of certain alkaloids (ajamalicine, papaverine, cinchonine, piperine, berberine) and some plant materials containing alkaloids (Berberis aristata, Solanum nigrum, and Piper longum) were determined. The method was compared with other methods. It can be used for routine analysis of commercial samples by industries dealing with herbal drugs for standardization of plant materials containing alkaloids and for alkaloid-containing pharmaceutical products.

179 citations


Journal ArticleDOI
TL;DR: Of 108 pesticides/metabolites tested, 104 showed sufficient stability in most matrixes for determination by LC/MS/MS, and belong to 20 chemical classes, which demonstrate the general applicability of the method for multiclass analysis.
Abstract: A method was developed for screening crops for a range of pesticide residues by liquid chromatography/tandem mass spectrometry (LC/MS/MS). A complete set of LC, electrospray ionization (ESI), and tandem MS acquisition parameters was established for the determination of 108 analytes; these parameters were used for the simultaneous acquisition of 98 analytes in the positive ESI mode and 10 analytes in an additional MS/MS method in the negative ESI mode. The entire procedure involves extraction of residues with methanol-water and partition into dichloromethane. The utility of the method is demonstrated by the analysis of crops of 5 matrix types (water-containing, acidic, dry, sugar-containing, and fatty). Of 108 pesticides/metabolites tested, 104 showed sufficient stability in most matrixes for determination by LC/MS/MS. These analytes belong to 20 chemical classes, which demonstrate the general applicability of the method for multiclass analysis. By using matrix-matched standards, 67 compounds could be determined in most matrixes with recoveries of 70-120% and a relative standard deviation of < or = 25% at the 0.01 mg/kg level.

152 citations


Journal ArticleDOI
TL;DR: The history, use, and analytical methods for the most commonly used indicator organisms, including the aerobic plate count, yeasts and molds, the coliform groups, are summarized.
Abstract: Indicator organisms have been used for nearly a century to assess the microbiological status of water and foods. Beginning with their use in water sanitation programs, their applications have been extended over the years to other products, and they have become important components of the microbiological testing programs of both industry and regulatory agencies. Functionally, they may be viewed as safety or quality indicators. Safety indicators suggest the presence of conditions associated with increased risk of exposure to a pathogen. Quality indicators assess conditions of importance to product manufacture or consumer acceptability. This minireview summarizes the history, use, and analytical methods for the most commonly used indicator organisms, including the aerobic plate count, yeasts and molds, the coliform groups,

100 citations


Journal ArticleDOI
TL;DR: The proposed method is simple, rapid, and specific for monitoring residues of chloramphenicol, thiamphen Nicol, florfenicol, and florfanicol amine in a number of aquatic species and compares favorably with those obtained by established LC methodology.
Abstract: A liquid chromatographic (LC)/mass spectrometric (MS) method was developed for determining the residues of chloramphenicol, thiamphenicol, florfenicol, and florfenicol amine in a number of aquatic species. The phenicols are extracted with acetone, the extracts are partitioned with dichloromethane, the aqueous layer is removed, and the organic layer is evaporated to dryness. The residue is dissolved in dilute acid and defatted with hexane, and the aqueous layer is prepared for analysis by LC. The phenicols are determined by reversed-phase LC by using a Hypersil C18-BD column with a water-acetonitrile gradient and MS detection using selected-ion recording. Calibration curves were linear for all analytes between 0.015 and 0.425 ng injected. The relative standard deviations for measurements by the proposed method were < 10% for all of the analytes studied, with recoveries ranging from 71% for florfenicol amine to 107% for florfenicol in salmon tissue spiked at the 2 ng/g level. Detection limits of 0.1 ng/g for florfenicol and chloramphenicol, 0.3 ng/g for thiamphenicol, and 1.0 ng/g for florfenicol amine are easily obtainable. The operational errors, interferences, and recoveries for spiked samples compare favorably with those obtained by established LC methodology. The proposed method is simple, rapid, and specific for monitoring residues of chloramphenicol, thiamphenicol, florfenicol, and florfenicol amine in a number of aquatic species.

91 citations


Journal ArticleDOI
TL;DR: An amplified enzyme-linked immunosorbent assay (amp-ELISA) was compared with the AOAC Official Method 977.26 for detection of Clostridium botulinum and its toxins in foods and found it could be used to screen suspect cultures for botulinal toxins.
Abstract: An amplified enzyme-linked immunosorbent assay (amp-ELISA) was compared with the AOAC Official Method 977.26 for detection of Clostridium botulinum and its toxins in foods. Eleven laboratories participated and the results of 10 laboratories were used in the study. Two anaerobic culture media, tryptone peptone glucose yeast extract (TPGY) and cooked meat medium (CMM) were used to generate toxic samples with types A, B, E, and F botulinal strains. Nonbotulinal clostridia were also tested. The toxicity of each botulinal culture was determined by the AOAC method, and the cultures were then diluted, if necessary, to high (about 10,000 minimal lethal dose [MLD]/mL) and low (about 100 MLD/mL) test samples. The overall sensitivity of detection in TPGY and CMM cultures with the amp-ELISA was 94.7% at about 100 MLD/mL and 99.6% for samples with > or = 10,000 MLD/mL toxicity. The amp-ELISA detection sensitivity for low toxin samples was 92.3% in TPGY and 99.4% in CMM. The false-positive rate ranged from 1.5% for type A to 28.6% for type F in TPGY, and from 2.4% for type A to 11.4% for type F in CMM. Most of the cross-reactivity was due to detection of other botulinal types, especially in high toxin samples. The amp-ELISA could be used to screen suspect cultures for botulinal toxins. Positive amp-ELISA samples would be confirmed by the AOAC reference method.

80 citations


Journal ArticleDOI
TL;DR: Uncertainty of measurement comprises, in general, many components that may be evaluated from the statistical distribution of the results of a series of measurements and can be characterized by experimental standard deviations.
Abstract: Uncertainty of measurement comprises, in general, many components. Some of these components may be evaluated from the statistical distribution of the results of a series of measurements and can be characterized by experimental standard deviations. The other components, which also can be characterized by standard deviations, are evaluated from assumed probability distributions based on experience or other information.

68 citations


Journal ArticleDOI
TL;DR: A simple liquid chromatography/mass spectrometry approach for the determination of widely used representatives of polar/thermolabile pesticides in fruits was developed and validated and Carbofuran was the only compound for which recovery was not satisfactory due to its loss in the SPE cleanup step.
Abstract: A simple liquid chromatography/mass spectrometry (LC/MS) approach for the determination of widely used representatives of polar/thermolabile pesticides in fruits was developed and validated The group of pesticides comprised benzimidazoles and azoles (carbendazim, thiabendazole, imazalil, propiconazole, prochloraz, epoxiconazole, flusilazole, tebuconazole, bitertanol); N-methylcarbamates (carbaryl, carbofuran, methiocarb); and phenylureas and benzoylphenylureas (linuron, diflubenzuron, triflumuron, teflubenzuron, flufenoxuron) Matrixes (apple, apricot) were extracted with acetonitrile and crude extracts were cleaned up by solid-phase extraction (SPE) using either mixed cation exchange or hydrophilic lipophilic balance cartridges LC separation of pesticides was performed on a reversed-phase column, Discovery C18 Electrospray ionization and ion trap MS/MS detection were applied For most pesticides, overall recoveries ranged from 75 to 122%, and repeatability (as relative standard deviation) from 5 repetitive determinations of recovery ranged from 3 to 21% Carbofuran was the only compound for which recovery was not satisfactory due to its loss in the SPE cleanup step Limits of detection were 01-3 microg/kg for benzimidazole and azole fungicides and carbamate insecticides For urea insecticides, detection limits were slightly higher (3-10 microg/kg)

64 citations


Journal ArticleDOI
TL;DR: A peer-verified method is presented for the determination of percent moisture and fat in meat products by microwave drying and nuclear magnetic resonance (NMR) analysis.
Abstract: A peer-verified method is presented for the determination of percent moisture and fat in meat products by microwave drying and nuclear magnetic resonance (NMR) analysis. The method involves determining the moisture content of meat samples by microwave drying and using the dried sample to determine the fat content by NMR analysis. Both the submitting and peer laboratories analyzed 5 meat products by using the CEM SMART system (moisture) and the SMART Trac (fat). The samples, which represented a range of products that meat processors deal with daily in plant operations, included the following: (1) fresh ground beef, high-fat; (2) deboned chicken with skin; (3) fresh pork, low-fat; (4) all-beef hot dogs; and (5) National Institute of Standards and Technology Standard Reference Material. The results were compared with moisture and fat values derived from AOAC-approved methods, 950.46 (Forced Air Oven Drying) and 960.39 (Soxhlet Ether Extraction).

61 citations


Journal ArticleDOI
TL;DR: A method was developed to identify and simultaneously quantify Clenbuterol-like substances with anilinic moieties and drugs with phenolic and catecholic moieties, such as Ractopamine and Zilpaterol, in retinal tissue and results are discussed in terms of a multiresidue approach to improve reliability of the monitoring strategy.
Abstract: Adrenergic drugs for growth promotion have been outlawed in European meat production; however, molecules such as Ractopamine and Zilpaterol are licensed for feeding swine and cattle in the United States, Mexico, and South Africa. Analysis of bovine retinal extracts has recently shown considerable extension in the detection period following withdrawal. Previous studies demonstrated that residual concentrations of Clenbuterol and related substances in retinal tissue were > 100 ng/g at day 50 of withdrawal. A method was developed to identify and simultaneously quantify Clenbuterol-like substances with anilinic moieties and drugs with phenolic and catecholic moieties, such as Ractopamine and Zilpaterol, in retinal tissue. The method was validated according to SANCO/1805/2000. After extraction in 0.1 N HCl, samples were cleaned up on C18 non-endcapped solid-phase extraction columns and analyzed as trimethylchlorosilane derivatives by gas chromatography/tandem mass spectrometry, electron impact mode. At concentrations of agonists between 62.5 and 250.0 ng/g in bovine retina, mean recoveries ranged from 85.3 to 94.8%, repeatability was < 9.6%, and within-laboratory reproducibility was < 10.5%. The decision limits (CCalpha) were within the range of 66.3-70.4 ng/g, and the detection capability (CCbeta) varied from 73.9 to 79.8 ng/g. Results are discussed in terms of a multiresidue approach to improve reliability of the monitoring strategy.

Journal ArticleDOI
TL;DR: The LC method is suitable for routine use in fruit products and foods containing > 5 mg/100 g vitamin C and is recommended for further validation by AOAC INTERNATIONAL and International Fruit Juice Union.
Abstract: A interlaboratory study was conducted to evaluate a liquid chromatographic (LC) procedure for the determination of total vitamin C in foods at levels of 5-60 mg/100 g. Emphasis was placed on fruit juices, although selected foods were also included in the study. Following dissolution of sample in water, endogenous dehydroascorbic acid was converted to ascorbic acid by precolumn reduction with dithiothreitol at neutral pH. Total ascorbate was determined by C18 reversed-phase LC with a phosphate eluent at pH 2.5, incorporating dithiothreitol to maintain vitamin C in the reduced form, and UV detection at 254 nm. Seven types of fruit juices and foods were tested by 19 collaborators in 7 countries. Three duplicate juices and foods met the criteria for Youden pairs and yielded repeatability relative standard deviation of 5.80-14.66%. Reproducibility relative standard deviation ranged from 6.36 to 35.54% (n = 10) with HORRAT values of 0.82-4.04. The LC method is suitable for routine use in fruit products and foods containing > 5 mg/100 g vitamin C and is recommended for further validation by AOAC INTERNATIONAL and International Fruit Juice Union.

Journal ArticleDOI
TL;DR: A method for quantifying florfenicol amine (FFA) in channel catfish muscle was validated according to U.S. Food and Drug Administration guidelines and should yield a more accurate estimate of the total florfanicol-related residue level in muscle tissue from florfinicol-treated catfish than could be achieved by solvent extraction alone.
Abstract: A method for quantifying florfenicol amine (FFA) in channel catfish muscle was validated according to U.S. Food and Drug Administration guidelines. FFA is the proposed marker residue for the veterinary antibiotic florfenicol in catfish muscle for regulatory surveillance purposes. The method includes acid hydrolysis followed by sample cleanup with ethyl acetate extraction, basification, solid-phase extraction, and quantitation by liquid chromatography with UV detection. The assay was validated at 5 concentrations in the range of 0.075-35 microg/g muscle. The overall mean recovery of FFA from fish tissues fortified at these concentrations ranged from 85.7 to 92.3%, 4.8-17.2% relative standard deviation (RSD). The assay limit of detection was 0.044 microg/g muscle based on analysis of control muscle. Catfish muscle samples containing incurred florfenicol residues were analyzed in quintuplicate with RSD < 5%. Acid hydrolysis has previously been demonstrated to convert florfenicol and its known metabolites to FFA and to release a significant amount of FFA from nonextractable florfenicol residues in tissues containing incurred residues in other species. By using acid hydrolysis, this method should yield a more accurate estimate of the total florfenicol-related residue level in muscle tissue from florfenicol-treated catfish than could be achieved by solvent extraction alone.

Journal ArticleDOI
TL;DR: This paper provides a comprehensive concept for evaluating validation parameters for planar Chromatographic fingerprinting by considering the stationary phase, sample application, developing solvent, chromatogram development, plate labeling, derivatization, documentation, and chromatographic equipment.
Abstract: In herbal medicinal products the entire herbal drug or an herbal drug preparation is regarded as the active pharmaceutical ingredient, regardless of whether constituents with defined therapeutic activity are known. In quality control and stability testing of herbal medicinal products, fingerprint chromatograms are used as powerful tools to evaluate and compare the composition of compounds in such products. To fulfill the International Conference on Harmonization and Good Manufacturing Practice-based regulatory requirements in pharmaceutical quality control, chromatographic fingerprint analysis needs to be validated. Based on a standardized methodology, this paper provides a comprehensive concept for evaluating validation parameters for planar chromatographic fingerprinting by considering the stationary phase, sample application, developing solvent, chromatogram development, plate labeling, derivatization, documentation, and chromatographic equipment. Validation parameters addressed include stability of the analyte, selectivity, robustness testing, and method reproducibility.

Journal ArticleDOI
TL;DR: The rapid method developed for the evaluation of forskolin was successful in the qualitative and quantitative evaluation of the marker compound in C. forskohlii plant material and in market products claiming to contain C.Forskolin.
Abstract: A rapid method was developed for the evaluation of forskolin in Coleus forskohlii Briq (Lamiaceae) Forskolin was quantitated in the root and stem of dried C forskohlii and in 17 market products by reversed-phase liquid chromatography (LC) with a photodiode array detector at 210 nm The temperature was held constant at 30 degrees C, and the retention time of forskolin was approximately 68 min The samples were extracted with acetonitrile by sonication The precision of the method was confirmed by a standard deviation < 50% (n = 3), and forskolin recovery was 991% Limit of detection was 15 microg/mL, and the response was linear through zero from 63 to 630 microg/mL with a correlation coefficient (R2) of 09998 Identity of the marker compound was confirmed by an LC/mass spectrometry experiment The method was successful in the qualitative and quantitative evaluation of the marker compound in C forskohlii plant material and in market products claiming to contain C forskohlii

Journal ArticleDOI
TL;DR: The method of standard additions was found to be necessary to avoid matrix effects in the quantification of fungicide residues and showed that concentrations of the fungicides identified in grapes were lower than the MRLs established by the European legislation.
Abstract: A new analytical method, based on organic solvent extraction with dichloromethane-acetone (75 + 25, v/v) followed by gas chromatography with mass spectrometric detection, is presented for the determination of residues of 10 fungicides in white grapes for vinification. Some of them (cyprodinil, fludioxonil, and pyrimethanil) have been used for only 2-3 years and, therefore, no methods are available in the scientific literature for such a screening. Quality parameters yielded good precision (relative standard deviation of <10%) and detection limits (ranging between 1 and 18 microg/kg) that are lower than the maximum residue limits (MRLs) set by the 76/895/European Economic Community (EEC) and 90/642/EEC Directives. The applicability of the method was evaluated by analysis of 5 different white grapes produced in the Rias Baixas area in Galicia (northwestern Spain) for vinification. The method showed good performance in analyses of real samples to determine whether the concentrations of the fungicides used exceeded their MRLs. The method of standard additions was found to be necessary to avoid matrix effects in the quantification of fungicide residues. Results showed that concentrations of the fungicides identified in grapes were lower than the MRLs established by the European legislation.

Journal ArticleDOI
TL;DR: The developed method allows the accurate and rapid determination of low levels of fosetyl-Al residues in lettuce with very little sample handling and good sensitivity; it was shown to be robust by the analysis of almost 100 samples.
Abstract: This paper describes a new method for the sensitive and selective determination of fosetyl-aluminum (Al) residues in vegetable samples. The method involves extraction with water by using a high-speed blender and subsequent injection of the 5-fold diluted extract into the liquid chromatograph. Fosetyl-Al is determined by liquid chromatography with electrospray tandem mass spectrometry after the addition of tetrabutylammonium acetate as the ion-pairing reagent. The method has been used to assay lettuce samples spiked at 2 and 0.2 mg/kg. Recoveries were satisfactory, with mean values of 98 and 106%, respectively, and relative standard deviations were <10%. The limit of quantitation was 0.2 mg/kg, and the limit of detection was as low as 0.05 mg/kg. Matrix-matched calibration was used for quantitation, and the addition of an internal standard improved repeatability. The developed method allows the accurate and rapid determination of low levels of fosetyl-Al residues in lettuce with very little sample handling and good sensitivity; it was shown to be robust by the analysis of almost 100 samples.

Journal ArticleDOI
TL;DR: A gas chromatographic method was developed for the simultaneous determination of 12 pyrethroids in tomato puree, peach nectar, orange juice, and canned peas using a miniaturized extraction-partition procedure requiring small amounts of nonchlorinated solvents.
Abstract: A gas chromatographic method was developed for the simultaneous determination of 12 pyrethroids (tefluthrin, bifenthrin, fenpropathrin, cyhalothrin, permethrin, cyfluthrin, cypermethrin, alpha-cypermethrin, flucythrinate, fenvalerate, fluvalinate, and deltamethrin) in tomato puree, peach nectar, orange juice, and canned peas. A miniaturized extraction-partition procedure requiring small amounts of nonchlorinated solvents is used. Samples are extracted with acetone, partitioned with ethyl acetate-cyclohexane (50 + 50, v/v), and cleaned up on a Florisil cartridge. The final extract is analyzed by gas chromatography with both electron capture and mass spectrometric detection modes. Studies at fortification levels of 0.010-0.100 mg/kg gave mean recoveries ranging from 70.2 to 96.0% and coefficients of variation between 4.0 and 13.9% for all compounds. Quantitation limits were < 0.010 mg/kg for electron capture detection.

Journal ArticleDOI
TL;DR: An automated biosensor surface-plasmon resonance-based assay was developed for the determination of immunoglobulin G (IgG) in bovine milk and colostrum with either goat or rabbit antibovine IgG or protein G used as detecting molecule and compared with independent alternative methods.
Abstract: An automated biosensor surface-plasmon resonance-based assay was developed for the determination of immunoglobulin G (IgG) in bovine milk and colostrum with either goat or rabbit antibovine IgG or protein G used as detecting molecule. The method is configured as a direct and nonlabeled immunoassay, with quantitation against an authentic IgG calibrant. Whole colostrum or milk is prepared for analysis by dilution into buffer. Analysis conditions, including ligand immobilization, flowrate, contact time, and regeneration, were optimized, and nonspecific binding was evaluated. Performance parameters included working range of 15-10 000 ng/mL, method detection limit of 0.08 mg/mL, overall instrument response reproducibility relative standard deviation (RSD(R)) of 0.47%, mean between-run RSD(R) of 10.5% for colostrum, and surface stability over 200 analyses. The proposed method was compared with independent alternative methods. The technique was applied to the measurement of IgG content during early lactation transition from colostrum to milk, as well as in consumer milk, colostrum, and hyperimmune milk powders.

Journal ArticleDOI
TL;DR: A gas chromatographic procedure was developed for the assay of 2-hydroxy-4-methoxybenzaldehyde in both fresh and dried roots of different origin, and steam hydrodistillation was suitable for extraction of the volatile oils.
Abstract: The roots of Decalepis hamiltonii and Hemidesmus indicus are aromatic and possess the crystalline compound 2-hydroxy-4-methoxybenzaldehyde as the major compound (> 90%) in their volatile oils. A gas chromatographic procedure was developed for the assay of 2-hydroxy-4-methoxybenzaldehyde in both fresh and dried roots of different origin. Benzyl butyrate was used as the internal standard. Among the methods tried, steam hydrodistillation was suitable for extraction of the volatile oils. The quantity of this aromatic compound varied from 0.03 to 0.54%.

Journal ArticleDOI
TL;DR: The method showed acceptable within- and between-laboratory precision for this matrix, as evidenced by HORRAT values, at the target levels of determination for aflatoxin B1.
Abstract: A collaborative study was conducted to evaluate the effectiveness of an immunoaffinity column cleanup liquid chromatography (LC) method for determination of aflatoxin B1 in cattle feed at a possible future European regulatory limit (1 ng/g). The test portion was extracted with acetone-water (85 + 15), filtered, diluted with water, and applied to an immunoaffinity column. The column was washed with water to remove interfering compounds, and the purified aflatoxin B1 was eluted with methanol. Aflatoxin B1 was separated and determined by reversed-phase liquid chromatography (RP-LC) and detected by fluorescence after post column derivatization (PCD) involving bromination. PCD was achieved with either pyridinium hydrobromide perbromide (PBPB), used by 14 laboratories, or an electrochemical cell and addition of bromide to the mobile phase, used by 7 laboratories. Both derivatization techniques were not significantly different when compared by the t-test; the method was statistically evaluated for all laboratories together (bromination and PBPB). The cattle feed samples, both spiked and naturally contaminated with aflatoxin B1, were sent to 21 laboratories in 14 different countries (United States, Japan, and Europe). Test portions were spiked at levels of 1.2 and 3.6 ng/g for aflatoxin B1. Recoveries ranged from 74 to 157%. Based on results for spiked samples (blind pairs at 2 levels) as well as naturally contaminated samples (blind pairs at 3 levels), the relative standard deviation for repeatability (RSDr) ranged from 5.9 to 8.7%. The relative standard deviation for reproducibility (RSDR) ranged from 17.5 to 19.6%. The method showed acceptable within- and between-laboratory precision for this matrix, as evidenced by HORRAT values, at the target levels of determination for aflatoxin B1. No major differences in RSD were observed, showing that the composition of the feeds was not a factor for the samples tested and that the method was applicable for all materials used.

Journal ArticleDOI
TL;DR: A rapid confirmatory liquid chromatographic/tandem mass spectrometic method was developed for determination of chloramphenicol in bovine milk and the detection capability related to the transition product of lowest abundance was 0.03 microg/kg.
Abstract: A rapid confirmatory liquid chromatographic/tandem mass spectrometic method was developed for determination of chloramphenicol in bovine milk. Chloramphenicol was extracted directly from milk by solid-phase extraction on a C18 cartridge. The extract was further cleaned up on neutral aluminium oxide. Three transition products were monitored in negative ion mode after atmospheric pressure chemical ionization. The detection capability related to the transition product of lowest abundance was 0.03 microg/kg. The mean recovery was 90% at levels of 0.1-0.2 microg/kg. The relative repeatability standard deviations were 4.3, 3.8, and 2.8% at levels of 0.1, 0.2, and 1.0 microg/kg, respectively.

Journal ArticleDOI
TL;DR: It is recommended that ISO 6579:2002 culture method for Salmonella be adopted Official First Action for the analysis of fresh cheese, fresh chilled and frozen poultry, and dried egg products.
Abstract: Three food types were analyzed for the presence of Salmonella by the AOAC culture method and by the International Organization for Standardization (ISO 6579:2002) culture method. Paired test portions of each food type were simultaneously analyzed by both methods. A total of 21 laboratories representing federal government agencies and private industry, in the United States and Europe, participated in this interlaboratory study. Foods were artificially contaminated with Salmonella and competing microflora if naturally contaminated sources were not available. No statistical differences (p < 0.05) were observed between the AOAC and ISO culture methods for fresh cheese and dried egg products. A statistically significant difference was observed for one of the 2 lots of poultry from the first trial. The poultry meat used in this run was radiation sterilized, artificially contaminated with Salmonella and competitive flora, and then lyophilized. A second trial was conducted with 2 separate lots of raw ground chicken that were naturally contaminated. The results from the second trial showed no statistical difference between the 2 culture methods. A third trial involving 4 laboratories was conducted on 2 separate lots of naturally contaminated raw poultry. Again, no statistically significant differences occurred. It is recommended that ISO 6579:2002 culture method for Salmonella be adopted Official First Action for the analysis of fresh cheese, fresh chilled and frozen poultry, and dried egg products.

Journal ArticleDOI
TL;DR: The SPFIA test can be used as an alternative to classical inhibition tests and for post-screening inhibitor- positive kidneys, because it detects 3 specific groups of antibiotics, which enables selection of specific confirmatory methods for identification and quantification.
Abstract: Parallux, a solid-phase fluorescence immunoassay (SPFIA) developed for antibiotic residue detection in milk, was used for analysis of bovine and porcine kidney tissue. Four tetracyclines, 2 broad-spectrum cephalosporins, 3 beta-lactam antibiotics, and cephapirin were detected in one run after minimal sample preparation. This commercially available test system is designed as cartridges, each with a combination of 1-4 tests. One cartridge can be used to detect 4 analytes in the same sample, or 1 or 2 analytes in different samples. The cartridge with the combination tetracyclines-ceftiofur-penicillin-cephapirin was selected because tetracyclines, beta-lactam antibiotics as well as cephalosporins, are registered for oral or parenteral use in bovines and pigs in Europe. The test is qualitative and is recommended only for screening. Tetracycline, oxytetracycline, chlortetracycline, and doxycycline were easily detected at 300 ppb with the tetracyclines channel; ceftiofur at 1000 ppb and cefquinome at 200 ppb with the ceftiofur channel; penicillin G, ampicillin, and amoxicillin at 50 ppb with the penicillin channel; and cephapirin at 100 ppb with the cephapirin channel. These levels are equal to or lower than the corresponding maximal residue limits in kidney tissue. Cephalexin was not detected. The SPFIA test can be used as an alternative to classical inhibition tests and for post-screening inhibitor- positive kidneys, because it detects 3 specific groups of antibiotics, which enables selection of specific confirmatory methods for identification and quantification.

Journal ArticleDOI
TL;DR: A method was developed, using commercially available immunoaffinity chromatography cleanup cartridges, followed by detection by gas chromatography/mass spectrometry, to screen for residues of the hormone growth promotants diethylstilbestrol, dienestrol, hexestrol; and zeranol in bovine urine.
Abstract: A method was developed, using commercially available immunoaffinity chromatography cleanup cartridges, followed by detection by gas chroma- tography/mass spectrometry, to screen for resi- dues of the hormone growth promotants diethyl- stilbestrol, dienestrol, hexestrol, and zeranol in bovine urine. The single-laboratory, in-house vali- dation included assessment of recoveries, repeat- ability, linearity of response, detection capability, and specificity (cross-reactivity) with a suite of an- tibiotics and other hormonal growth promotants. The method was validated for screening at a target concentration of 2.0 g/L in urine. The detection capabilities for the analytes were diethylstilbestrol, 0.24; dienestrol, 0.15; hexestrol, 0.84; and zeranol, 0.28 g/L. food animals is banned in the European Union (EU), and no residues of these substances are allowed in meat products sold there. To meet EU requirements, cattle producers in a number of exporting countries have developed "hormone-free cattle" programs, where animals are certified to have been grown to market weight without the use of HGPs. National authorities are required to collect and test bovine urine for the presence of these HGPs in order to demonstrate that cattle raised for ex- port to the EU are free of these substances (2, 3). For cattle to be acceptable to the EU, the HGPs must not be detectable in urine by a method capable of detecting residues at a concen- tration of 2.0 g/L or higher (4). This level defines the mini- mum required performance limit (MRPL) for the analytical method. To meet the EU regulations, the Canadian Food In- spectionAgency(CFIA)requiredasuitablescreeningmethod for these HGPs in bovine urine. An existing CFIA method for DES, DIEN, HEX, and ZER in tissue, based on a method by Covey et al. (5), was extended to bovine urine. The original gas chromatography/mass spec- trometry(GC/MS)determinationoftheanalyteswasretained, and a new sample preparation methodology, based on com- mercially available immunoaffinity chromatography (IAC) columns, was incorporated into the method. This approach was adopted to minimize the amount of time and resources needed to develop and validate the method, and reduce famil- iarization time for the technical staff. The new screening method was validated for the reliability of detection of the analytes at a concentration of 2.0 g/L in fortified blank urine samples. The single-laboratory, in-house validation included assessment of recoveries, repeatability, linearity of response, detection capability (CC), and selectivity. METHOD

Journal ArticleDOI
TL;DR: A method was developed to detect both toxins in corn and wheat by liquid chromatography/mass spectrometry of an extract of ground grain, which requires no sample cleanup and can detect the toxins at 0.05 microg/g.
Abstract: The fungus Fusarium graminearum is a pathogen of both wheat and corn. Strains of the fungus from the United States produce a toxin, deoxynivalenol (DON); strains of the fungus from Asia and Europe produce DON or a related toxin, nivalenol. These toxins can cause disease in livestock, and their po­ tential presence in feed and foods is a concern for animal and human health. A method was devel­ oped to detect both toxins in corn and wheat by liquid chromatography/mass spectrometry of an extract of ground grain. The method requires no sample cleanup and can detect the toxins at

Journal ArticleDOI
Zhao-Yang Li1, Zhichao Zhang1, Qi-Lin Zhou1, Qing-Min Wang1, Ruyu Gao1, Qin-Sun Wang1 
TL;DR: The proposed method is rapid, precise, and sensitive, and is appropriate for the investigation of the stereo- and enantioselective degradation of pesticides in environmental media.
Abstract: The separation of enantiomers and diastereomers of 8 commonly used pesticides was investigated by liquid chromatography (LC) using a Chiralcel OD column (cellulose tris-3,5-dimethylphenylcarbamate as the chiral stationary phase) and a Pirkle-type Chirex 3020 column (urea derivative from the reaction of (R)-1-(alpha-naphthyl)ethylamine with (S)-tert-leucine, chemically bonded to 3-aminopropylsilanized silica as the chiral stationary phase). The pesticides studied included one organophosphorus insecticide (phenthoate), 3 triazole fungicides (uniconazole, diniconazole, and propiconazole), and 4 pyrethroids (fenpropathrin, beta-cypermethrin, beta-cyfluthrin, and alpha-fenvalerate). The enantiomers were separated within 20 min with a resolution of > or = 1.5 using a mixture of n-hexane and 2-propanol as the mobile phase for all the pesticides studied except propiconazole, for which only the 2 diastereomers were baseline separated. This method allows determination of the enantiomers or stereoisomers of the above pesticides in soil. The strategy was as follows: (1) First, the total concentration(s) of the enantiomer pair(s) of a chiral pesticide in soil was (were) determined by a newly developed matrix solid-phase dispersion (MSPD) procedure, followed by silica-based LC quantification. The recoveries ranged from 76.5 to 93.6% with relative standard deviations of 6.0%. (2) Second, the enantiomeric ratio(s) (ER(s)) of the chiral pesticide was (were) determined by LC with a chiral stationary phase after fractionation of the MSPD extract by silica-based LC. The determined ERs or stereoisomeric ratio(s) (SR(s); for propiconazole, only the SR of the 2 diastereomers was determined) in soil samples spiked with the above 8 racemic pesticides agreed with those of the corresponding standard solutions. (3) Third, based on the total concentrations and the corresponding ERs, the concentration of each enantiomer in soil was calculated. The proposed method is rapid, precise, and sensitive, and is appropriate for the investigation of the stereo- and enantioselective degradation of pesticides in environmental media.

Journal ArticleDOI
TL;DR: A liquid chromatographic method with post-column derivatization and fluorescence detection is proposed because of its sensitivity and specificity.
Abstract: A simple and accurate cleanup procedure using polymeric sorbent was developed for the determination of oxytetracycline (OTC) and tetracycline (TC) residues in salmon muscle. It was applied to the analysis of 20 salmon samples during a month period. The OTC and TC residues were extracted with ethylenediaminetetracetic acid (EDTA)–McIlvaine buffer acidified at pH 4.0 and cleaned up by solid-phase extraction with a polymeric sorbent. The advantages of the polymeric sorbent over the silica-based sorbent in the cleanup of salmon muscle samples are described. A liquid chromatographic method with post-column derivatization and fluorescence detection is proposed because of its sensitivity and specificity. The average recoveries of OTC and TC from muscle salmon tissue fortified at 50, 100, and 200 g/kg levels, ranged from 83.9 to 93.4% with a coefficient of variation between 4.09 and 5.80%. The limit of quantitation for OTC and TC in salmon muscle was 50 g/kg.

Journal ArticleDOI
TL;DR: A multiresidue method was developed for the de termination of 16 polycyclic aromatic hydrocarbons (PAHs) in unifloral and multifloral honeys with low consumption of organic solvents.
Abstract: A multiresidue method was developed for the de termination of 16 polycyclic aromatic hydrocarbons (PAHs) in unifloral and multifloral honeys. The analytical procedure is based on the matrix solid-phase dispersion of honey on a mixture of Florisil and anhydrous sodium sulfate in small glass columns and extraction with hexane-ethyl acetate (90 + 10, v/v) with assisted sonication. The PAH residues are determined by gas chromatography with mass spectrometric detection using selected-ion monitoring. Average recoveries for all the PAHs studied were in the range of almost 80 to 101%, with relative standard deviations of 6 to 15%. The limits of detection ranged from 0.04 to 2.9 microg/kg. The simultaneous extraction and cleanup of samples makes this method simple and rapid, with low consumption of organic solvents

Journal ArticleDOI
TL;DR: The simplicity, sensitivity, and enhanced kinetics of the new antagonism cell bioassay format provide the basis for development of a practical alternative to conventional mouse testing for PSP.
Abstract: Although cytotoxicity assays provide several advantages over mouse bioassays, sodium channel-blocking marine toxins, such as those associated with paralytic shellfish poison (PSP), require prolonged incubation periods of 24-48 h. This is in marked contrast to in vitro detection of sodium channel-enhancing marine toxins such as ciguatoxins or brevetoxins which can be accomplished in as few as 4-6 h. We developed a modified PSP cell bioassay that is as rapid as in vitro methods for sodium channel-enhancing toxins. The cell bioassay is based on a saxitoxin-dependent antagonism of the rapid in vitro effects of brevetoxin or ciguatoxin. Comparative analysis of naturally incurred PSP residues by both antagonism cell bioassay and the mouse bioassay demonstrated significant correlation. The simplicity, sensitivity, and enhanced kinetics of the new antagonism cell bioassay format provide the basis for development of a practical alternative to conventional mouse testing for PSP.