Biosynthetic origin of geosmin in red beets (Beta vulgaris L.)

Geosmin provides the characteristic but sometimes undesirable "earthy" flavor to red table beets. To date, it is not known whether geosmin is a byproduct of beet metabolism or synthesized by soil-borne microorganisms and taken up by the beets during maturation. Analysis of mature beet roots revealed that peels contained 6 times the amount of geosmin compared to the bodies and cores. Sterilized beet seeds were aseptically grown in a basal medium prior to analysis for the presence of geosmin. Using a headspace solid-phase microextraction (HSPME) method, the relative recovery of geosmin from beet seedling extracts was 72.0 +/- 4.2% with (-)-menthone as the internal standard. The presence of geosmin in aseptically grown beet seedlings was confirmed by gas chromatography-mass spectrometry using authentic geosmin as the standard. During aseptic growth, the concentration of geosmin in seedlings remained constant for up to 5 months but increased at 6 months. Geosmin added to the growth medium was not absorbed by the seedlings. These studies support the conclusion that red beets are capable of endogenous synthesis of geosmin.     

Determination of 2-methylisoborneol and geosmin produced by Streptomyces sp. and Anabaena PCC7120

A new sample preparation and enrichment technique, headspace liquid-phase microextraction (HS-LPME) linked to gas chromatography-mass spectrometry (GC-MS), was developed for the determination of the off-flavor odorants, 2-methylisoborneol and geosmin, produced by Streptomyces sp. and Anabaena PCC7120. Some of the factors that influence the extraction efficiency of HS-LPME, such as the type of extraction solvent, ionic strength of sample solution, and sample agitation rate, were studied and optimized by a single factor test. Other factors, including extraction temperature, extraction time, microdrop volume, and headspace volume were optimized by orthogonal array design. Extraction of 2-methylisoborneol and geosmin was conducted by exposing 2.5 microL of 1-hexanol for 9 min at 50 degrees C in the headspace of a 20 mL vial with a 10 mL of sample solution saturated by NaCl and stirred at 800 rpm. The developed protocol demonstrated good repeatability (relative standard deviations (RSDs) < 5%), wide linear ranges (10-5000 ng/L, r2 > 0.999), and low limits of detection (LODs) for 2-methylisoborneol and geosmin (0.05 ng/L for both analytes). Subsequently, the method was successfully applied to extract the analytes in bacterial cultures with high recoveries (from 94% to 98%). Compared with headspace solid-phase microextraction (HS-SPME), HS-LPME demonstrates better linearity, precision, and recovery. Importantly, the sensitivity is about 1 order of magnitude higher than that of most HS-SPME. The results showed that HS-LPME coupled with GC-MS is a simple, convenient, rapid, sensitive, and effective method for the qualitative and quantitative analysis of 2-methylisoborneol and geosmin.     

Improved malonaldehyde assay using headspace solid-phase microextraction and its application to the measurement of the antioxidant activity of phytochemicals

A modified malonaldehyde (MA) assay for antioxidant activity, which involves derivatization and headspace solid-phase microextraction (HS-SPME) was developed and validated. The recovery of MA as 1-methylpyrazole (product of MA and N-methylhydrazine) from a headspace of an aqueous solution containing MA, buffer, surfactant, and cod liver oil using HS-SPME with a PDMS/DVB fiber was 91.3 +/- 3.38%. MA was analyzed by a gas chromatograph with a nitrogen-phosphorus detector, and its detection limit was 0.0103 nmol/mL. The antioxidant activities of natural compounds were determined as the percentage inhibition of MA formed from cod liver oil oxidized by Fenton's reagents in the above aqueous solution. Sesamol inhibited MA formation most (86.1%), followed by eugenol (84.4%), capsaicin (80.7%), ethylvanillin (45.3%), and vanillin (31.6%) at a level of 50 microg/mL. This method did not require any organic solvents and is a simple, fast, and a highly sensitive method for MA determination.     

Determination of geosmin, 2-methylisoborneol, and a musty-earthy odor in wheat grain by SPME-GC-MS, profiling volatiles, and sensory analysis

Geosmin and 2-methylisoborneol-compounds responsible for the musty-earthy off-odor of wheat grain, were isolated by SPME and analyzed by GC-MS. Carboxen/PDMS/DVB fiber coating was selected because of its highest extraction efficiency. Concentrations of geosmin and 2-methylisoborneol as low as 0.001 microg/kg were detected in SIM mode using ion trap mass spectrometer. Apart from GC-MS determination of geosmin and 2-methylisoborneol, various methods for evaluating the musty-earthy off-odor caused by these compounds in wheat grain are presented. Sensory profile analysis differentiated wheat grain into sound and off-flavored, but the method was tedious. Similar groupings, however, were obtained using more rapid methods such as comparison of volatile profiles using SPME-fast GC with PCA projection of data and metal oxide (MOS) based electronic nose.     

Headspace solid phase microextraction applied to the analysis of organophosphorus insecticides in strawberry and cherry juices

A method based on a headspace solid phase microextraction (HS-SPME) technique followed by gas chromatography with flame thermionic and mass spectrometric detection was developed for the determination of seven organophosphorus (OPs) insecticide residues in strawberry and cherry juice samples. The extraction capacities of four fiber coatings, polyacrylate (PA 85 microm), poly(dimethylsiloxane) (PDMS 100 microm), carbowax-divinylbenzene (CW-DVB 65 microm), and poly(dimethylsiloxane)-divinylbenzene (PDMS-DVB 65 microm), have been studied and compared. The method was developed using spiked strawberry and cherry juices in a concentration range of 0.5-50 microg/L. The PDMS 100 microm fiber showed good extraction efficiency for the target compounds. An increase in the extraction efficiency of OP insecticides was observed when the parameters affecting the HS-SPME process such as temperature, extraction time, salt additives, stirring rate, pH, and effect of dilution were optimized. Good linearity of compounds was observed in the tested concentration range. The relative standard deviations were found to be <20%. The limits of detection were between 0.025 and 0.050 microg/L. The mean relative recoveries ranged from 82 to 102%.     

Evaluation of fumonisin contamination in cornflakes on the Belgian market by "flow-through" assay screening and LC-MS/MS analyses

A total of 205 cornflake samples collected in Belgian retail stores during 2003-2004 were surveyed for the natural occurrence of fumonisin B1 (FB1), B2 (FB2), and B3 (FB3). These cornflake samples, originating from conventional as well as from organic production, were analyzed using an intralaboratory-validated LC-MS/MS method. Additionally, 90 cornflake samples were subjected to rapid screening using a flow-through enzyme immunoassay method to demonstrate the practicability of a screening test coupled to a validated confirmatory LC-MS/MS method for the management of food safety risks. FB(1) concentrations ranged from not detected (nd) [LOD (FB1) = 20 microg/kg] to 464 microg/kg with mean and median concentrations of respectively 104 +/- 113 and 54 microg/kg. For FB2 and FB3, the concentration ranges varied respectively from nd [LOD (FB2) = 7.5 microg/kg] to 43 microg/kg and from nd [LOD (FB3) = 12.5 microg/kg] to 90 microg/kg. Mean concentrations for FB2 and FB3 were respectively 12 +/- 8 and 21 +/- 15 microg/kg, while the median concentration was 11 microg/kg for FB2 and 19 microg/kg for FB3. From the statistical tests (chi2 and ANOVA model III), it could be concluded that the agricultural practice did not have any significant effect on the fumonisin concentrations but that the variation between different batches was significant (p < 0.0001).     

氮肥施用量对高产甜菜纤维根系分布及活力的影响

为了解施N肥对甜菜生长的影响规律。在田间条件下,研究了不同施N量（0、90、180、270、360 kg/hm2）对甜菜（KWS2409）纤维根系生长、分布和活力变化的影响。结果表明,施N比对照增加浅层侧根数、外层和深层纤维根干重及100 cm土层纤维根总干重,并提高各生育期侧根和主根活力。其中,100 cm土层最大纤维根干重施N 比对照增加了60.4%～168.4%,最大侧根数增加了22.7%～75.1%,且以0—20 cm和40—60 cm深的外土层及80—100 cm深的内土层纤维根系增加较大,分别比对照增加了129.6%～266.8%、71.0%～234.0%和101.5%～202.8%。主根伤流液量和侧根的活力分别比对照增加了56.2%～89.9%、23.7%～63.4%。N 180 kg/hm2处理0—100 cm土层中纤维根总量、各土层中根量最大,各生育时期主根和侧根活力最强,块根产量（82609.63 kg/hm2）和产糖量（13892.64 kg/hm2）均最高,而含糖率（16.83%）较N0处理（18.34%）略降。说明合理施N量有利于甜菜纤维根系生长和提高产糖量。     

Chemical and sensory quantification of geosmin and 2-methylisoborneol in rainbow trout (Oncorhynchus mykiss) from recirculated aquacultures in relation to concentrations in basin water

Globally, aquaculture systems with water recirculation experience increasing problems with microbial taste and odor compounds (TOCs) such as geosmin and 2-methylisoborneol (MIB). This study investigated the content of geosmin and MIB in water and the flesh of 200 rainbow trouts from eight recirculated aquaculture systems in Denmark. TOC content in the fish flesh was measured by a dynamic headspace extraction method and was evaluated by a sensory panel. The results showed significant correlations between TOC content in water and fish and between chemical analysis and sensory perception. When geosmin exceeded 20 ng/L in the water, 96% of the fish had an intense muddy flavor, but below 10 ng geosmin/L, 18% of the fish (only 3% in special depuration ponds) had an intense muddy flavor. The results indicate that TOC levels <10 ng/L will ensure that a negligible portion of the fish obtains an unpalatable taste and flavor due to TOCs.     

Analysis of acrylamide in a complex matrix of polyacrylamide solutions treated by heat and ultraviolet light

A recently developed headspace/solid-phase microextraction/gas chromatograph (GC) equipped with a nitrogen-phosphorus detector (NPD) (HS/SPME/GC/NPD) method was used to analyze acrylamide formed in an aqueous polyacrylamide solution (25%) treated by heat or photo-irradiation. Original polyacrylamide contained 0.43 +/- 0.11 microg/mL of acrylamide. When polyacrylamide solution was heated at 70 degrees C for 16 h with 0.5% potassium persulfate, the amount of acrylamide increased to 1.02 +/- 0.11 microg/mL. When polyacrylamide solution was irradiated by UV (lambda = 300 nm) for 16 h with 0.05% 2-anthraquinone sulfate sodium salt, the amount of acrylamide increased to 1.14 +/- 0.54 microg/mL. Polyacrylamide has been used in cosmetic formulations. The present study, therefore, suggests that there is another route of acrylamide exposure to humans in addition to foods and beverages.     

High-performance liquid chromatographic method for the quantitative determination of Hypoxoside in African potato (Hypoxis hemerocallidea) and in commercial products containing the plant material and/or its extracts

Hypoxoside is a norlignan diglucoside present in the corms of African potato (Hypoxis hemerocallidea). The latter is used as a popular African traditional medicine for it's nutritional and immune-boosting properties. A reverse phase high-performance liquid chromatography method was developed and validated for the determination of hypoxoside using a mobile phase consisting of acetonitrile:water (20:80, v/v). The method was linear throughout the range of 10-100 microg/mL and provided a high degree of accuracy (100 +/- 4%). The recovery of the method was found to be 100 +/- 5%, and the precision of the study, % relative standard deviation intraday and interday (over three separate days), was better than 6.15 and 5.64%, respectively. The limits of detection and quantification were calculated to be 0.75 and 3.5 microg/mL, respectively. This method was applied to the analysis and quality control of African potato corms as well as 12 commercially available products. The daily intake of hypoxoside through traditionally prepared African potato decoction was also evaluated.     

Analysis of alternariol and alternariol monomethyl ether on flavedo and albedo tissues of tangerines (Citrus reticulata) with symptoms of alternaria brown spot

A method was developed for the quantification of alternariol and alternariol monomethyl ether on tangerines with and without symptoms of Alternaria brown spot disease. The method employs solid-phase extraction for cleanup, followed by high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS) for detection. This method was validated on flavedo (exocarp or epicarp, exterior yellow peel) and on albedo tissue (mesocarp, interior white peel). An excellent linearity over a range of 0.50-20.0 mg/kg was achieved, with r2 >or= 0.997. The limits of detection (LOD) and quantification (LOQ) were fewer than 0.13 and 0.50 microg/kg, respectively. The relative standard deviations (RSDs) were 相似文献   

High-affinity monoclonal antibodies for detection of the microbial metabolite, 2-methylisoborneol

The production of 2-methylisoborneol (MIB) by certain fungi and algae can contribute musty off-flavors to foods and water supplies if uncontrolled. The goal of this research was to develop a nonsensory simple method for the detection of MIB. Anti-MIB monoclonal antibodies were produced by immunizing mice with borneol-conjugated protein and selecting positive clones with an MIB-protein conjugate. An indirect competitive immunoassay developed using this antibody had a detection limit of 0.6 microg L(-)(1) and an I(50) value of 5 microg L(-)(1). Detection was relatively specific for MIB and showed 20% cross-reactivity with borneol or isoborneol and 4-5% cross-reactivity with camphor. No cross-reactivity to geosmin was observed.     

Aflatoxin and fumonisin contamination of commercial corn (Zea mays) hybrids in Mississippi

Resistance to mycotoxin contamination was compared in field samples harvested from 45 commercial corn (maize) hybrids and 5 single-cross aflatoxin-resistant germplasm lines in years with high and moderate heat stress. In high heat stress, mycotoxin levels were (4.34 +/- 0.32) x 10(3) microg/kg [(0.95-10.5 x 10(3) microg/kg] aflatoxins and 11.2 +/- 1.2 mg/kg (0-35 mg/kg) fumonisins in commercial hybrids and 370 +/- 88 microg/kg (140-609 microg/kg) aflatoxins and 4.0 +/- 1.3 mg/kg (1.7-7.8 mg/kg) fumonisins in aflatoxin-resistant germplasm lines. Deoxynivalenol was detected (one-fourth of the samples, 0-1.5 mg/kg), but not zearalenone. In moderate heat stress, mycotoxin levels were 6.2 +/- 1.6 microg/kg (0-30.4 microg/kg) aflatoxins and 2.5 +/- 0.2 mg/kg (0.5-4.8 mg/kg) fumonisins in commercial hybrids and 1.6 +/- 0.7 microg/kg (0-7 microg/kg) aflatoxins and 1.2 +/- 0.2 mg/kg (0.5-3.0 mg/kg) fumonisins in aflatoxin-resistant germplasm lines. The results are consistent with heat stress playing an important role in the susceptibility of corn to both aflatoxin and fumonisin contamination, with significant reductions of both aflatoxins and fumonisins in aflatoxin-resistant germplasm lines.     

Determination of flubendazole and its metabolites in eggs and poultry muscle with liquid chromatography-tandem mass spectrometry

The optimization of a quantitative and sensitive LC-MS/MS method to determine flubendazole and its hydrolyzed and reduced metabolites in eggs and poultry muscle is described. The benzimidazole components were extracted from the two matrices with ethyl acetate after the sample mixtures had been made alkaline. The HPLC separation was performed on an RP C-18 column with gradient elution, using ammonium acetate and acetonitrile as mobile phase. The analytes were detected after atmospheric pressure electrospray ionization on a tandem quadrupole mass spectrometer in MS/MS mode. The components were measured by the MS/MS transition of the molecular ion to the most abundant daughter ion. The overall extraction recovery values for flubendazole, the hydrolyzed metabolite, and the reduced metabolite in eggs (fortification levels of 200, 400, and 800 microg kg(-1)) and muscle (fortification levels of 25, 50, and 100 microg kg(-1)) were, respectively, 77, 78, and 80% and 92, 95, and 90%. The trueness (fortification levels of 400 and 50 microg kg(-1), respectively, for eggs and muscle), expressed as a percentage of the added values for these analytes, was, respectively, 89, 100, and 86 and 110, 110, and 98%. The proposed MS detection method operating in the MS/MS mode is very selective and very sensitive. The limits of detection for flubendazole and its hydrolyzed and reduced metabolites in egg and muscle were, respectively, 0.19, 0.29, and 1.14 microg kg(-1) and 0.14, 0.75, and 0.31 microg kg(-1). The limits of quantification were, respectively, 1, 1, and 2 microg kg(-1) and 1, 1, and 1 microg kg(-1). The discussed method was applied to a pharmacokinetic study with turkeys. Residue concentrations in breast and thigh muscle of turkeys orally treated with flubendazole were quantified. Medicated feed containing 19.9 and 29.6 mg kg(-1) flubendazole was provided to the turkeys for seven consecutive days. For the trial with the recommended dose of 19.9 mg kg(-1), one day after the end of the treatment, the mean sum of the flubendazole plus hydrolyzed metabolite residue values in thigh and breast muscle declined to below the maximum residue limit (50 microg kg(-1)) and were, respectively, 36.6 and 54.1 microg kg(-1). The corresponding values with the higher dose of 29.6 mg kg(-1) were, respectively, 101.7 and 119.7 microg kg(-1).     

Determination of pesticides and PCBs in virgin olive oil by multicolumn solid-phase extraction cleanup followed by GC-NPD/ECD and confirmation by ion-trap GC-MS

A multicolumn solid-phase extraction cleanup for the determination of organophosphorus (OP) and organochlorine (OC) pesticides plus PCB congeners in virgin olive oil is presented. The method involves dissolution of the olive oil in hexane, followed by a cleanup system using a diatomaceous earth column (Extrelut-QE) with reversed (C(18)) and normal (alumina) phase SPE columns. Determination of OPs was by GC-NPD, while the OCs and PCBs were analyzed using GC-ECD. Recovery assays for OPs varied from 81.7% to 105.3%, for OCs ranged between 74.3% and 99.4%, while for PCBs were from 60.1% to 119.2%. Quantitation limits ranged from 10 to 25 microg/kg olive oil for OPs, and from 1 to 6 microg/kg olive oil for OCs and PCBs. In the case of positive samples, the confirmation of pesticide identity was performed by ion-trap GC-MS/MS. The applicability of the method was assayed with 19 virgin olive oil samples collected from different olive mills of Aragón (Spain). Only one OP pesticide (acephate) was detected in one sample at a concentration of 10 microg/kg. Organochlorine pesticides were found in 5-47% of samples at very low levels ranging from 1.5 to 5.2 microg/kg. PCBs were found in 20-90% of samples, showing concentrations between 2.3 and 17.3 microg/kg.     

Application of gas chromatography coupled to triple quadrupole mass spectrometry for the multiresidue analysis of pesticides in olive oil

A new multiresidue method has been developed and validated for the simultaneous determination of 100 pesticide residues in olive oil. The determination of pesticide residues was carried out in only 19 min by gas chromatography coupled to tandem mass spectrometry using a triple quadrupole mass analyzer. The mass spectrometer was operated in electron ionization and the selection reaction monitoring mode was used, acquiring two or three fragmentation reactions per compound. Two extraction processes were studied, and an evaluation of the stability and sensitivity of the chromatographic system has been performed for the tested extraction procedures. The final proposed methodology was based on a liquid-liquid partition with an n-hexane/acetonitrile mixture followed by a gel permeation chromatography cleanup step. An adequate lineal relation was obtained in the studied concentration range (10-200 microg kg (-1)); the recovery values were in the range 70-110% for the two levels of concentration studied: 12 and 50 microg kg (-1). Precision values, expressed as relative standard deviation, were lower than 18% at the aforementioned spiking levels; detection limits, confirmation limits, and quantitation limits were below or equal to 1.9, 2.6, and 3.6 microg kg (-1), respectively. The developed methodology was applied to the analysis of pesticide residues in real samples of olive oil from the south of Spain.     

Toxicokinetics, recovery, and metabolism of metamitron in goat

Toxicokinetic behavior and metabolism studies of metamitron and its effect on the cytochrome P(450) content of liver microsomal pellet were carried out in black Bengal goats after a single oral administration at 278 mg kg(-1) and consecutive oral administration of 30 mg kg(-1) for 7 days. Metamitron was detected in the blood sample at 0.08 h (12.0 +/- 0.87 microg mL(-1)), maximum at 4 h (84.3 +/- 8.60 microg mL(-1)) and minimum (14.6 +/- 1.67 microg mL(-1)) at 36 h blood sample after a single oral administration. The absorption rate constant was 0.69 +/- 0.09 h(-1). The Vd(area) (2.00 +/- 0.08 L kg(-1)) and t(1/2)beta (8.98 +/- 0.70 h) values suggested wide distribution and long persistence of the compound in the body. The values of T approximately B (0.80 +/- 0.04), F(c) (0.55 +/- 0.01), Cl(B) (0.15 +/- 0.00 L kg(-1) h(-1)), and K(21) (0.41 +/- 0.03 h(-1)) suggested that metamitron retained in the blood compared to that in the tissue. Maximum concentration of metamitron residue was found in the adrenal gland followed by bile on day 4 of single oral administration. The higher Cl(R) compared to Cl(H) value indicated the excretion of the major portion (34-40%) through urine compared to feces (20-26%). Maximum concentrations of metamitron and its metabolite, deaminometamitron, were excreted through urine and feces at 48 and 24 h samples, respectively. The recovery of metamitron including its metabolite in terms of parent compound varied from 69.3 to 80.1%, of which contribution of metabolite in terms of parent compound varied from 53.1 to 63.0%. Repeated oral administration of metamitron at 30 mg kg(-1) for 7 days caused induction of the cytochrome P(450) content of liver microsomal pellet of goat, suggesting oxidative deamination of metamitron.     

Direct determination of paclobutrazol residues in pear samples by liquid chromatography-electrospray tandem mass spectrometry

A rapid and sensitive liquid chromatography/electrospray ionization/tandem mass spectrometry (LC-ESI-MS-MS) method has been developed for the determination of the plant growth regulator paclobutrazol in pear samples. Extraction was performed with methanol by using a high-speed blender Ultra-Turrax, and 10 microL of pear extract was directly injected in the LC-ESI-MS-MS system without any previous sample treatment. The highest sensitivity of the method was achieved under MS-MS conditions obtaining a limit of detection of 0.7 microg/kg and a quantification limit of 5 microg/kg, with a run time of only 5.5 min. Recoveries for paclobutrazol from spiked pear samples at 0.005, 0.05, and 0.5 mg/kg were around 82-102% with relative standard deviations between 2 and 7%. The method was applied to real treated and untreated samples of pears, using quality control samples as a evaluation of the method reliability. Two MS-MS transitions were selected, one for quantification (294 > 70) and the other for confirmation of the analyte (296 > 70). All the experiments were performed in compliance with good laboratory practices.     

Analysis of four 5-nitroimidazoles and their corresponding hydroxylated metabolites in egg, processed egg, and chicken meat by isotope dilution liquid chromatography tandem mass spectrometry

An isotope dilution liquid chromatography-electrospray ionization-tandem mass spectrometry method is presented for the simultaneous analysis of several 5-nitroimidazole-based veterinary drugs, which are dimetridazole (DMZ), ronidazole (RNZ), metronidazole (MNZ), ipronidazole (IPZ), and their hydroxylated metabolites (DMZOH, MNZOH, and IPZOH), in egg (fresh egg, whole egg powder, and egg yolk powder) and chicken meat. Data acquisition was achieved by applying multiple reaction monitoring, and quantitation was performed by means of five deuterated internal standards (ISs), namely, DMZ-d3, RNZ-d3, IPZ-d3, DMZOH-d3, and IPZOH-d3, whereas MNZ and MNZOH were quantitated using DMZOH-d3. At the lowest fortification levels (i.e., 0.5 microg/kg for fresh egg and chicken meat and 1.0 microg/kg for other egg-based matrices) and for compounds having their own corresponding deuterated analogue used as an IS, acceptable performance data were obtained (corrected recoveries, 88-111%; decision limits, 0.07-0.36 microg/kg; detection capabilities, 0.11-0.60 microg/kg; and within-lab precision, < or = 15%). The method failed to give acceptable quantitative results for MNZ and MNZOH due to the unavailability of the corresponding deuterated ISs. Nevertheless, a reliable identification of these two analytes at levels < or = 1 microg/kg was still feasible.     

Application of manual and automated systems for purification of ochratoxin a and zearalenone in cereals with immunoaffinity columns.

A manual vacuum manifold and an automated solid phase extraction (ASPEC) system were applied for purification of ochratoxin A and zearalenone in wheat, rye, barley, and oat samples with immunoaffinity columns followed by separation with a high-performance liquid chromatograph and fluorescence detection. The immunoaffinity columns for manual sample purification were purchased from a different manufacturer than were those for the automated system. The limit of detection (LOD) for the method for ochratoxin A with a vacuum manifold and ASPEC was 0.1 microg/kg. For the method for zearalenone, the LODs were 1.5 microg/kg with a vacuum manifold and 3 microg/kg with ASPEC. For the methods for ochratoxin A at spiking levels of 0.6 and 2.5 microg/kg, mean recoveries for different cereals varied from 68 to 106%. For the methods for zearalenone, mean recoveries varied from 78 to 117% at spiking levels of 9 and 25 microg/kg. The relative standard deviations of repeatability with various cereals employing both methods were 2-15 and 2-19% for ochratoxin A and zearalenone, respectively.