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1.
In October and November 2004, 91 spice samples (70 ground red pepper, six black pepper, five white pepper, five spice mix and five chilli samples), the majority of which originated from commercial outlets, were analysed for aflatoxins B1, B2, G1 and G2 (AFB1, AFB2, AFG1, AFG2) and ochratoxin A (OTA) content by high-performance liquid chromatography (HPLC) after immunoaffinity column clean-up. Eighteen of the 70 ground red pepper samples contained AFB1, seven of them in a concentration exceeding the 'maximum level' of 5 µg kg-1 (range 6.1-15.7 µg kg-1). Of the other spices assayed, the AFB1 contamination of one chilli sample exceeded 5 µg kg-1 (8.1 µg kg-1). Thirty-two of the 70 ground red pepper samples contained OTA, eight of them in a concentration exceeding the 10 µg kg-1 'maximum level' (range 10.6-66.2 µg kg-1). One chilli sample was contaminated with OTA at 2.1 µg kg-1. The AFB1 and OTA contamination of ground red pepper exceeding the 'maximum level' (5 and 10 µg kg-1, respectively) was obviously the consequence of mixing imported ground red pepper batches heavily contaminated with AFB1 and OTA with red pepper produced in Hungary. This case calls attention to the importance of consistently screening imported batches of ground red pepper for aflatoxin and ochratoxin A content and strictly prohibiting the use of batches containing mycotoxin concentrations exceeding the maximum permitted level.  相似文献   

2.
Three hundred and twenty samples from the 1999 UK harvest comprising wheat (201 samples), barley (106) and oats (13) were analysed for ochratoxin A and deoxynivalenol. A small number of organic samples was also obtained. Samples were collected from farms, central stores, mills, maltings and ports from across the UK from February to April 2000. Ochratoxin A and deoxynivalenol analysis was by affinity column clean up and high-performance liquid chromatography with fluorescence and ultraviolet light detection, respectively, with limits of detection of 0.2 and 20 μg kg-1. The survey found ochratoxin A at below 5 μg kg-1 in 97% of the samples indicating satisfactory storage conditions. The remaining 3% of the samples contained ochratoxin A at levels between 5.2 and 231 μg kg-1, but none of these samples was intended for human consumption. Deoxynivalenol was detected in 88% of all samples, with 83% below 100 μg kg-1; the maximum level was 600 μg kg-1. Twenty samples containing deoxynivalenol at or above 150 μg kg-1 by high-performance liquid chromatography were all confirmed by gas chromatography/mass spectrometry. Nivalenol was also detected by gas chromatography/mass spectrometry at levels of 50 μg kg-1 or higher in 18 of 20 samples where deoxynivalenol was confirmed.  相似文献   

3.
A total of 208 samples of commercial pasteurized milk gathered from retail outlets across Japan during the winter season were analysed for aflatoxin M1 (AFM1). Japan was divided into 11 regions from north to south, and nine to 45 milk samples from each region were randomly purchased between December 2001 and February 2002. Each milk sample was cleaned up by an immunoaffinity column, and AFM1 was quantified by liquid chromatography with fluorescence detection in four independent laboratories. The limit of detection of the method was 0.001 μg kg-1. The identity of the putative AFM1 in milk sample was confirmed by the formation of AFM1 hemi-acetal with trifluoroacetic acid. Based on the results obtained with spiked samples (0.05 μg AFM1 kg-1), the mean recovery was 91.4%, the relative standard deviation for repeatability was 4.6%, and the relative standard deviation for reproducibility was 8.0% among four independent laboratories. AFM1 was detected in 207 (99.5%) of 208 milk samples at 0.001-0.029 μg kg-1, with a mean of 0.009 μg kg-1 and a 90th percentile of 0.014 μg kg-1. No significant difference of the level of AFM1 contamination was observed among the regions.  相似文献   

4.
Australian survey of acrylamide in carbohydrate-based foods   总被引:2,自引:0,他引:2  
A method was developed and validated for the determination of acrylamide in carbohydrate-based foods. Solid-phase extraction employing a mixed-bed anion and cation exchange cartridge in series with a C18 extraction disk was used to clean-up water extracts of food samples before analysis by liquid chromatography coupled with tandem mass spectrometry detection. The limit of detection was calculated as approximately 25 μg kg-1 and the limit of reporting was 50 μg kg-1. The average method recovery for 84 samples from a range of matrices reporting was 99% with a relative standard deviation of 11.2%. A survey was conducted of 112 samples of carbohydrate-based foods composited from 547 products available in the Australian market. The analytical results were used in conjunction with Australian food consumption data derived from the 1995 National Nutrition Survey (NNS) to prepare preliminary dietary exposure estimates of Australians to acrylamide through only the food groups examined. Mean dietary exposure to acrylamide resulting from consumption of the foods tested, for Australians aged 2 years and above, was estimated as 22-29 µg day-1 (equivalent to 0.4-0.5 µg kg-1 bodyweight day-1) and between 73 and 80 µg day-1 (1.4 and 1.5 µg kg-1 bodyweight day-1) for 95th percentile consumers. Young children (2-6 years) consuming acrylamide-containing foods had a higher acrylamide exposure on a per kilogram bodyweight basis (mean 1.0-1.3 µg kg-1 bodyweight day-1). The estimated exposure of Australians to acrylamide is similar to that estimated for other countries.  相似文献   

5.
A method for the simultaneous quantitative determination of deoxynivalenol (DON), fumonisin B1 (FB1) and zearalenone (ZEN) in maize by liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry (LC-APCIMS/MS), using stable isotopically labelled and structural analogues internal standards, is described. The procedure involves accelerated solvent extraction followed by two solid-phase clean-up steps on strong anion exchange resin and a Mycosep® column. Typical recoveries were calculated by spiking blank maize at three different concentrations for deoxynivalenol (200, 400 and 1000 μg kg-1) at 70%, for fumonisin B1 (100, 200 and 1000 μg kg-1) at 90%, and for zearalenone (50, 100 and 200 μg kg-1) at 40%. LC-APCIMS/MS analyses were realized in collision-induced dissociation on an ion-trap instrument to provide a high degree of selectivity and sensitivity. Extraction of ions from two transition reactions, monitored by LC-APCIMS/MS for each analyte, enabled a limit of detection for DON, FB1 and ZEN at, respectively, 10, 20 and 3 μg kg-1, and a limit of quantification at, respectively, 50, 50 and 10 μg kg-1. The robustness of the method was also evaluated with the analysis of wheat samples.  相似文献   

6.
The results of surveillance for ochratoxin A (OTA) in 1885 samples of sultanas taken during five crop years between 1999 and 2003 are reported. The analytical method was based on extraction with methanol + sodium bicarbonate and clean-up by immunoaffinity column chromatography followed by high-performance liquid chromatography with fluorescence detection. The limit of detection for OTA was 0.3 µg kg-1. The results show that 9.3% of the samples contained no detectable levels of OTA, whereas 0.6% had concentrations exceeding 10 µg kg-1; the remaining 90.3% had levels within the range 0.3-10 µg kg-1. The overall mean OTA concentration in the total number of 1885 samples taken was 1.36 ± 2.91 µg kg-1; the overall median was calculated as 0.90 µg kg-1.  相似文献   

7.
A method for the determination of malachite green and its major metabolite leucomalachite green in rainbow trout muscle is reported with limits of detection of 0.8 and 0.6 μg kg-1, respectively. Residues were extracted with an acetonitrile-acetate buffer mixture and partitioned into methylene chloride. Clean-up of the extracts was performed on alumina and propylsulfonic acid solid-phase extraction columns using the automated solid-phase extraction system. The chromatographic separation of malachite green and leucomalachite green was achieved on a Chromspher 5B column using an acetonitrile-acetate buffer mobile phase. Leucomalachite green was converted to malachite green by post-column oxidation before spectrophotometric detection at 600 nm. The mean recoveries of malachite green and leucomalachite green from control rainbow trout muscle spiked at 2-50 μg kg-1 were 65% (range 63.4-65.9%, relative standard deviation 3.9-16.1%) and 74% (range 58.3-82.6%, relative standard deviation 3.3-11.4%), respectively. Qualitative confirmation of the determined residues was performed with liquid chromatography coupled with tandem mass spectrometry detection with limits of detection of 2.5 and 1 μg kg-1 for malachite green and leucomalachite green, respectively.  相似文献   

8.
A simple and rapid method is reported for the routine determination 1-phenylazo-2-naphthol (Sudan I) in chilli powder and in chilli-containing food products. The method involved Soxtec extraction from the products followed by high-pressure gel permeation chromatographic clean-up collecting the appropriate fraction. Analysis of this fraction was by HPLC with UV/VIS detection. The limit of detection was 7 μg kg-1 and the limit of quantification was 13 μg kg-1. The identity of Sudan I in food products was established by electrospray LC/MS with MS/MS confirmation. From a small survey of 30 retail samples, 11 samples of crushed chilli, Italian pasta, chilli-snack and vegetable sauce contained levels of Sudan I ranging from 24 to 5591 μg kg-1.  相似文献   

9.
Maize samples collected from storage bins and feed mills in Northern Italy between 1995 and 1999 were surveyed for the occurrence of aflatoxin B1 (AFB1), zearalenone (ZEA), deoxynivalenol (DON) and fumonisin (FB1); further, ergosterol was analysed as a fungal growth marker. The incidence and mean content of AFB1 were generally low; nevertheless, a remarkable contamination was found in two samples (109 and 158 μg kg-1), while five others exceeded 20 μg kg-1. DON and ZEA mean levels were significantly higher in 1996 (2716 and 453 μg kg-1) with respect to the other years, when mean contents ranged from 7 to 30% and from 3 to 17%, respectively, expressed in per cent of 1996 contents. FB1 was present in all samples and was by far the most remarkable mycotoxin in Northern Italian maize, with the exception of samples from 1996. The average level was 3064 μg kg-1, 69.6% of samples resulted over 1000 μg kg-1 and 16.9% over 5000 μg kg-1. Significant correlations were found between ergosterol and the major mycotoxin(s) in each year (FB1 in 1995 and 1997-99; ZEA + DON in 1996). Consequently, ergosterol seems to be a good index of the toxicological quality of maize. Climatic conditions influenced the growth of different fungal species. In 1996, the first 20 days of October were extremely rainy; these weather conditions delayed the harvest until the first week of November and favoured the growth of DON and ZEA producing fungi and the synthesis of mycotoxins. On the contrary, the temperate and dry climate of the other years supported the growth of FB1-producing fungi.  相似文献   

10.
Acrylamide in Asian foods in Hong Kong   总被引:3,自引:0,他引:3  
About 400 food samples, mainly Asian foods available in Hong Kong, were tested for acrylamide by an LC-MS/MS method using [1, 2, 3-13C3]-acrylamide as surrogate. The acrylamide levels in the more commonly consumed food items in the food groups such as rice and rice products, noodles, bakery and batter-based products, were generally less than 60 μg kg-1. Higher levels were found in the food groups such as biscuit-related products and crisps. The highest levels were detected in potato crisps (1500-1700 μg kg-1). Lower levels were found in rye flour-based crisps (440 μg kg-1), followed by corn-based (65 to 230 μg kg-1) and wheat flour-based crisps (61-200 μg kg-1), and then rice flour-based crisps (15-42 μg kg-1). The acrylamide formation during deep frying of a wheat flour-based product, Chinese fried fritter, was studied. Deep-frying at 170°C resulted in gentle but steady rise in acrylamide content. A steep rise for frying at 210°C was recorded. The moisture content of the product decreased with frying time, but the fat content increased. It is proposed that the reaction for the formation of acrylamide was initiated on the surface and then penetrated into the interior of the food matrix by heat transfer via radiation/conduction and diffusion of hot oil.  相似文献   

11.
A validated high-performance liquid chromatography (HPLC) method with fluorescence detection for the quantitative analysis of ochratoxin A (OTA) in cocoa beans is described. OTA was extracted with methanol-3% sodium hydrogen carbonate solution and then purified with immunoaffinity columns before its analysis by HPLC. The validation of the analytical method was based on the following criteria: selectivity, linearity, limit of detection and quantification, precision (within- and between-day variability) and recovery, robustness and uncertainty. Detection and quantification limits were 0.04 and 0.1 μg kg-1, respectively. Recovery was 88.9% (relative standard deviation = 4.0%). This method was successfully applied to the measurement of 46 cocoa bean samples of different origins. A total of 63% of cocoa bean samples was contaminated with a level greater than the limit of detection. The means and medians obtained for cocoa bean were 1.71 and 1.12 μg kg-1, respectively. Surveillance controls should be set up in both crops and factories involved in transformation processes to avoid this mycotoxin in final products.  相似文献   

12.
In this study, microbiological tests for the detection of beta-lactam antibiotics in meat and meat products were evaluated. The traditional FPT (four plate test, containing Bacillus subtilis and Kocuria rhizophila), BsDA (Bacillus stearothermophilus disc assay) and a newly developed microbiological test, Premi®Test (containing Bacillus stearothermophilus) were included in the study. The limit of detection (LOD) of the Premi®Test was compared with the LOD of the traditional methods. The detection limits of the tests were determined by using beta-lactam antibiotic standards dissolved in meat juice, as well as meat tissue obtained from laying hens after experimental administration of amoxicillin. Positive samples, based on inhibition of growth of the organism in the test, were confirmed by high performance liquid chromatography (HPLC). Growth inhibition in the traditional tests is visible as a clear zone on the plate, whereas for Premi®Test, this is based on the absence of a colour change of the test. The LODs of antibiotics tested were as follows: Penicillin G (PENG) 5 µg kg-1, amoxicillin (AMOX) 10 µg kg-1, ampicillin (AMP) 25 µg kg-1, oxacillin (OXA) 30 µg kg-1, and cloxacillin (CLOX) 30 µg kg-1 on the plate with Bacillus stearothermophilus. Beta-lactam antibiotics can be detected also on one plate seeded with Kocuria rhizophila, although the LODs are higher: PENG 10 µg kg-1, AMOX 25 µg kg-1, AMP 30 µg kg-1, OXA 50 µg kg-1, and CLOX 50 µg kg-1. Premi®Test was performed according to the Standard Operating Procedure intended for detection of beta-lactam antibiotics in poultry tissues with following LODs: PENG 4 µg kg-1, AMOX 5 µg kg-1, AMP 5 µg kg-1, OXA 40 µg kg-1, CLOX 50 µg kg-1. All tests are able to detect beta-lactam antibiotics such as penicillin G, ampicillin, amoxicillin, oxacillin and cloxacillin below the maximum residue level (MRL). However, the detection limits of the Premi®Test for PENG, AMOX and AMP were below the limits of BsDA and the plate containing Kocuria rhizophila.  相似文献   

13.
A simple and feasible method is described for analysing nine mycotoxins in cheese matrix. The method involves liquid extraction followed by high performance liquid chromatographic separation and mass spectrometric detection of the analytes, and allows the determination of aflatoxins B1, B2, G1, G2 and M1, ochratoxin A, mycophenolic acid, penicillic acid and roquefortine C simultaneously. Average recoveries of the mycotoxins from spiked samples at concentration levels of 5-200 µg kg-1 ranged from 96-143%. Within-day relative standard deviations at these concentration levels varied from 2.3-12.1%. The limit of quantification for aflatoxin M1 was 0.6 µg kg-1 and for the other compounds 5 µg kg-1. The method developed was applied for analysing these mycotoxins in blue and white mould cheeses purchased from Finnish supermarkets. Roquefortine C was detected in all of the blue mould cheese samples in concentrations of 0.8-12 mg kg-1. One blue cheese contained also 0.3 mg kg-1 mycophenolic acid. The other investigated mycotoxins were absent in the samples.  相似文献   

14.
The occurrence of deoxynivalenol (DON) in Danish wheat flour was studied during the period 1998-2003 by either capillary gas chromatography with electron capture detection and liquid chromatography coupled to an ion trap mass spectrophotometer. A total of 151 samples were collected from mills and the retail market in Denmark. Contamination levels varied considerably from year-to-year with the highest concentrations occurring in samples from the 2002 harvest with mean and median concentrations of 255 and 300 µg kg-1, respectively. Compared to other harvest years, 2002 had the highest amount of precipitation around flowering time, i.e. from the end of June to the beginning of July covering weeks 25-27. The lowest average levels were found in samples from the 2001 harvest, where weeks 25-27 were dry compared with other harvest years. The highest value (705 µg kg-1) was obtained in a flour sample from the 2002 harvest, but none of the tested samples exceeded the maximum limit of 750 µg kg-1, which has been recently introduced by the European Commission for DON in flour used as raw materials in food products. Calculation of chronic or usual intake by a deterministic approach showed that intake did not exceed the TDI of 1 µg kg-1 bw day-1 either for the whole population or for children. A probabilistic approach also showed that intake in general was below the TDI, but intake for children in the 99% percentile amounted to more than 75% of the TDI. The highest intake is calculated to be 2.5 µg kg-1 bw day-1.  相似文献   

15.
The European Union Baby Food Directive (1999/39/EC), which came into force on 1 July 2002, set legal maximum residue levels at 0.01 mg kg-1 for all pesticides in baby foods. The combination of large volume-difficult matrix introduction (LV-DMI) with gas chromatography-time of flight-mass spectrometry (GC-TOF-MS), described herein, provides the analyst with a simple but rapid alternative GC-MS technique for the multiresidue analysis of pesticides in fruit-based baby foods. Samples were extracted with ethyl acetate in the presence of Na2SO4 and NaHCO3 and the crude extracts were analysed directly using LV-DMI-GC-TOF-MS. The best overall results (98 pesticides quantified satisfactorily at a spiking level of 0.01 mg kg-1) were obtained by analysis of concentrated extracts (2.5 g crop ml-1) using a 30-m column, with a chromatographic run time of 25 min. A good signal-to-noise ratio was obtained at the lowest calibrated level (0.0125 μg ml-1), with excellent linearity achieved over the range 0.0125-0.25 μg ml-1 (equivalent to 0.005-0.1 mg kg-1). Average recoveries for the analysis of five replicate determinations at a spiking level of 0.01 mg kg-1 were between 79 and 114% with relative standard derivations generally less than 20%.  相似文献   

16.
The aim of this study was to determine the levels of lead and cadmium in chicken, pork, beef, lamb and turkey samples (both meat and meat products), collected in the island of Tenerife (Spain). Lead and cadmium were measured by graphite furnace atomic absorption spectrometry (GFAAS). Mean concentrations of lead and cadmium were 6.94 and 1.68 µg kg-1 in chicken meat, 5.00 and 5.49 µg kg-1 in pork meat, 1.91 and 1.90 µg kg-1 in beef meat and 1.35 and 1.22 µg kg-1 in lamb meat samples, respectively. Lead was below the detection limit in turkey samples and mean cadmium concentration was 5.49 µg kg-1. Mean concentrations of lead and cadmium in chicken meat product samples were 3.16 and 4.15 µg kg-1, 4.89 and 6.50 µg kg-1 in pork meat product, 6.72 and 4.76 µg kg-1 in beef meat product and 9.12 and 5.98 µg kg-1 in turkey meat product samples, respectively. The percentage contribution of the two considered metals to provisional tolerable weekly intake (PTWI) was calculated for meat and meat products. Statistically significant differences were found for lead content in meats between the chicken and pork groups and the turkey and beef groups, whereas for cadmium concentrations in meats, significant differences were observed between the turkey and chicken, beef and lamb groups. In meat products, no clear differences were observed for lead and cadmium between the various groups.  相似文献   

17.
The migration of trimellitic acid and its esters from epoxy anhydride coatings was determined in simulants as well as in canned foods. The most appropriate simulant was a combination of EC simulants B and C: 2% acetic acid/10% ethanol in water. The average migration into food was 900 μg kg-1. This far exceeds the 50 μg kg-1 for which the safety of trimellitic acid and its anhydride is ensured and the Swiss legal limit (QM(T) of 5 mg kg-1 coating). Furthermore, much trimellitic acid migrated as (unidentified) esters, i.e. toxicological testing of free trimellitic acid is inadequate for the material that in reality migrates.  相似文献   

18.
The levels of formaldehyde (FA) and acetaldehyde (AA) in polyethylene terephthalate (PET) bottles and in commercial mineral water are reported. All the water samples bottled in Japan contained detectable levels of FA (10.1-27.9 μg l-1) and AA (44.3-107.8 μg l-1). Of 11 European bottled water samples, eight did not contain either FA or AA, while the remaining three had detectable levels of FA (7.4-13.7 μg l-1) and AA (35.9-46.9 μg l-1). In three North American bottled water samples, two contained FA (13.6 and 19.5 μg l-1) and AA (41.4 and 44.8 μg l-1), and one did not. Regardless of the region of origin, all the sterilized water samples contained FA and AA, whilst in contrast, none of the unsterilized water without carbonate contained FA or AA. Of the carbonated water samples, three contained FA and AA, and one did not. When fortified with FA and AA, the commercial water sample without otherwise detectable FA and AA was able to reduce levels, although the commercial water sample containing FA and AA could not. The presence of bacteria in the commercial water samples was investigated using an ATP-based bioluminescent assay and heterotrophic plate count method. The commercial water without FA and AA contained heterotrophic bacteria, whilst the commercial water with FA and AA did not contain detectable bacteria. It is suggested that in this case both FA and AA migrated from PET materials, but were subsequently decomposed by the heterotrophic bacteria in the unsterilized water.  相似文献   

19.
Mercury and cadmium concentrations were measured in the flesh and liver (or hepatopancreas) of albacore (Thunnus alalunga) and horned octopus (Eledone moschata) to establish whether the concentrations exceeded the maximum levels fixed by the European Commission. In both species, mercury and cadmium mean concentrations were higher in liver (albacore: mercury = 2.41 μg g-1 wet wt, cadmium = 9.22 μg g-1 wet wt; horned octopus: mercury = 0.76 μg g-1 wet wt, cadmium = 6.72 μg g-1 wet wt) than in flesh (albacore: mercury = 1.56 μg g-1 wet wt, cadmium = 0.05 μg g-1 wet wt; horned octopus: mercury = 0.36 μg g-1 wet wt, cadmium = 0.33 μg g-1). Mercury concentrations exceeding the prescribed legal limit of 1 μg g-1 wet wt were found in almost all albacore samples (flesh: 71.4%; liver: 85.7%). For horned octopus, concentrations above 0.5 μg g-1 wet wt were observed solely in hepatopancreas, while in flesh, the concentrations were below this limit in all the samples examined. Of the flesh samples of albacore, 42.8% exceeded the proposed tolerance for cadmium for human consumption, whilst for horned octopus, the established limit was not exceeded in any sample.  相似文献   

20.
Total mercury was measured in the edible portions of 244 selected fish and shellfish purchased in Canada at the retail level. By species, average mercury concentrations ranged from 0.011 μg g-1 for oysters to 1.82 μg g-1 for swordfish. The predatory fish contained the highest concentrations of mercury: swordfish (mean 1.82 μg g-1, range 0.40-3.85 μg g-1), marlin (1.43, 0.34-3.19 μg g-1), shark (1.26, 0.087-2.73 μg g-1), and canned, fresh and frozen tuna (0.35, 0.020-2.12 μg g-1). Levels of mercury in the fresh and frozen tuna contained a mean of 0.93 μg g-1 (range 0.077-2.12 μg g-1) and were substantially higher than in the canned tuna (0.15, 0.02-0.59 μg g-1). In the canned tuna, mercury concentrations varied with subspecies, with the highest average concentrations being found in Albacore tuna (mean 0.26 μg g-1, range 0.19-0.38 μg g-1) and the lowest (0.047, 0.025-0.069 μg g-1) in five samples for which the subspecies of tuna were not identified. Mean concentrations of mercury in swordfish and fresh and frozen tuna were up to three times higher than reported for the USA. Dietary intake estimations found that provided fresh and frozen tuna, marlin, swordfish or shark are consumed once a month or less, the dietary intakes of total mercury by women of child-bearing age, averaged over 1 month, would fall below the Joint FAO/WHO Expert Committee on Food Additives provisional tolerable weekly intake for total mercury. The current Canadian advisory to children and women of child-bearing age is to limit their consumption of fresh and frozen tuna, swordfish and shark to no more than one meal per month.  相似文献   

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