Validation of a commercial receptor kit Sulfasensor® Honey for the screening of sulfonamides in honey according to Commission Decision 2002/657/EC

The Sulfasensor® Honey kit is a receptor test dedicated to the screening of sulphonamide residues respectively in different matrices. The aim of this project was to evaluate and validate this kit according to the Community Reference Laboratory (CRL) guideline for the validation of screening methods to achieve the French control plan for honey. The test is robust, quick (90?min for 40 samples), easy to perform and easy to read. The false-positive rate was estimated to be 12.5%. The detection capabilities CCβ of the kit were lower than or equal to 25?µg?kg^?1 for sulfamethazine, sulfamerazine, sulfathiazole and sulfapyridine, and between 25 and 50?µg?kg^?1 for sulfadiazine and sulfadimethoxine, 150?µg?kg^?1 for sulfaquinoxaline, and 1000?µg?kg^?1 for sulfamethoxazole and sulfamethizole. Sulfanilamide was not detected by the kit. The kit was applicable to a wide variety of honeys (different floral and geographical origins, liquid or solid). This kit was used to implement the French control plan for the detection of antibiotic residues in honey in 2010 in parallel with an HPLC method. However, in 2011 the kit was replaced by an LC-MS/MS method for the screening and confirmation of sulfonamide residues in honey, which detects all the sulfonamides of interest.     

Validation of two ELISA kits for the screening of tylosin and streptomycin in honey according to the European decision 2002/657/EC

Antibiotics are mixed with the food of bees to fight against diseases. No maximum residue limits have been set for honey. Recommended concentrations (RCs) have been published by European Union Reference Laboratories for tylosin and streptomycin. The objective of this project was to select and validate enzyme-linked immunosorbent assay (ELISA) kits for the screening of tylosin and streptomycin/dihydrostreptomycin residues to be implemented in the French honey control plan. Four ELISA kits for tylosin and five ELISA kits for streptomycin were evaluated. At the end, one kit each was selected and validated for tylosin (TECNA AB620) and streptomycin (Europroxima). Both ELISA kits for tylosin and streptomycin are specific, robust, fast and easy-to-use tests. The detection capability CCβ of tylosin A was less than or equal to 10?µg?kg^?1 (half the RC). The CCβ of desmycosin (the hydrolysed product of tylosin A in acidic conditions) is approximately 200?µg?kg^?1, which is five times the RC for tylosin (20?µg?kg^?1). Thus, this kit is fit for the screening of tylosin A but is unsuitable to detect desmycosin. The detection capability CCβ of streptomycin was less than or equal to 10?µg?kg^?1 (one fourth the RC). The cross-reactivity with dihydrostreptomycin was equal to 136%. Both ELISA kits were applicable to a wide variety of honey (single flower and multiflower, different floral origins, different geographic origins, different consistencies [liquid or solid] and different colours).     

Screening methods for the detection of antibiotic residues in slaughter animals: comparison of the European Union Four-Plate Test,the Nouws Antibiotic Test and the Premi®Test (applied to muscle and kidney)

Microbial growth inhibition tests are widely used as the primary screening approach for the detection of antibiotic residues in slaughter animals. In this study we evaluated and compared the performance of the European Union Four-Plate Test (EU4pt), the Nouws Antibiotic Test (NAT), and a commercial ampoule test, the Premi®Test (applied to both muscle and kidney), by parallel analysis of 735 slaughter animals. The EU4pt only showed significant inhibition with two muscle samples containing 305?µg?kg^?1 doxycycline and 648?µg?kg^?1 tulathromycin, while an maximum residue limit (MRL) violation of 1100?µg?kg^?1 sulfamethazine remained unnoticed. Premi®Test-muscle only detected the sulfamethazine containing sample, all other (1.1%) suspect samples appeared false-positive results. The same test applied to kidney yielded 4.1% suspect samples, while the NAT screening (based on analysis of renal pelvis fluid) showed 4.9% suspect results. The vast majority of these samples contained tetracycline and/or aminoglycoside residues. Premi®Test-kidney appeared to be more sensitive to aminoglycosides than the NAT screening, which failed to detect an MRL violation of 870?µg?kg^?1 gentamicin in kidney. Detection of less than MRL levels of tetracycline residues by the NAT proved its suitability for this residue group. Whether Premi®Test is sufficiently sensitive for accurate tetracycline detection in kidney remains doubtful, although changing over to kidney definitely improved the suitability of Premi®Test for the detection of residues in slaughter animals.     

Rapid multi-class multi-residue method for the confirmation of chloramphenicol and eleven nitroimidazoles in milk and honey by liquid chromatography-tandem mass spectrometry (LC-MS)

A confirmatory method was developed to allow for the analysis of eleven nitroimidazoles and also chloramphenicol in milk and honey samples. These compounds are classified as A6 compounds in Annex IV of Council Regulation 2377/90 (European Commission 1990) and therefore prohibited for use in animal husbandry. Milk samples were extracted by acetonitrile with the addition of NaCl; honey samples were first dissolved in water before a similar extraction. Honey extracts underwent a hexane wash to remove impurities. Both milk and honey extracts were evaporated to dryness and reconstituted in initial mobile phase. These were then injected onto a liquid chromatography-tandem mass spectrometry (LC-MS/MS) system and analysed in less than 9 min. The MS/MS was operated in multiple reaction monitoring (MRM) mode with positive and negative electrospray ionization. The method was validated in accordance with Commission Decision 2002/657/EC and is capable of analysing metronidazole, dimetridazole, ronidazole, ipronidazole and there hydroxy metabolites hydroxymetronidazole, 2-hydroxymethyl-1-methyl-5-nitroimidazole, and hydroxyipronidazole. The method can also analyse for carnidazole, ornidazole, ternidazole, tinidazole, and chloramphenicol. A recommended level of 3 µg l^?1/µg kg^?1 for methods for metronidazole, dimetridazole, and ronidazole has been recommended by the Community Reference Laboratory (CRL) responsible for this substance group, and this method can easily detect all nitroimidazoles at this level. A minimum required performance level of 0.3 µg l^?1/µg kg^?1 is in place for chloramphenicol which the method can also easily detect. For nitroimidazoles, the decision limits (CCα) and detection capabilities (CCβ) ranged from 0.41 to 1.55 µg l^?1 and from 0.70 to 2.64 µg l^?1, respectively, in milk; and from 0.38 to 1.16 µg kg^?1 and from 0.66 to 1.98 µg kg^?1, respectively, in honey. For chloramphenicol, the values are 0.07 and 0.11 µg l^?1 in milk and 0.08 and 0.13 µg kg^?1 in honey. Validation criteria of accuracy, precision, repeatability, and reproducibility along with measurement uncertainty were calculated for all analytes in both matrices.     

Predicted dietary intake of selenium by the general adult population in Belgium

The total selenium content of about 800 food products purchased in Belgium was determined and combined with food records to determine the nutritional selenium status of Belgian people. The largest selenium concentrations (>1?mg?kg^?1) were found in Brazil nuts and offal, of which the consumption is limited. Usually consumed food groups with the highest selenium concentrations were fish and shellfish (0.2–0.9?mg?kg^?1), eggs, poultry meat, cheese, mushrooms and pasta (approximately 0.2?mg?kg^?1). The mean dietary selenium intake was calculated to be 60?µg?day^?1, which is at the lower end but within the range recommended by the Superior Health Council in Belgium (60–70?µg?day^?1), and adequate according to the 55?µg?day^?1 recommended by the Scientific Committee on Food (SCF) of the European Commission. The major sources of selenium intake are meat and meat products (31%), fish and shellfish (20%), pasta and rice (12%), and bread and breakfast cereals (11%).     

Survey of aflatoxins in maize tortillas from Mexico City

In Mexico, maize tortillas are consumed on a daily basis, leading to possible aflatoxin exposure. In a survey of 396 2-kg samples, taken over four sampling days in 2006 and 2007 from tortilla shops and supermarkets in Mexico City, aflatoxin levels were quantified by HPLC. In Mexico, the regulatory limit is 12?µg?kg^?1 total aflatoxins for maize tortillas. In this survey, 17% of tortillas contained aflatoxins at levels of 3–385?µg?kg^?1 or values below the limit of quantification (<LOQ) and, of these, 13% were >12?µg?kg^?1 and 87% were below the regulatory limit. Average aflatoxin concentrations in 56 contaminated samples were: AFB₁ (12.1?µg?kg^?1); AFB₂ (2.7?µg?kg^?1); AFG₁ (64.1?µg?kg^?1) and AFG₂ (3.7?µg?kg^?1), and total AF (20.3?µg?kg^?1).     

Isotope dilution-GC-MS/MS analysis of 16 polycyclic aromatic hydrocarbons in selected medicinal herbs used as health food additives

Medicinal herbs have a very important role in health protection and disease control, and have been used in health foods. Polycyclic aromatic hydrocarbons (PAHs) have carcinogenic, biological and mutagenic effects. In this paper, the content of 16?PAHs as representative contaminants in nine Chinese medicinal herbs, as additives for health foods, was investigated in order to ensure food safety from this source. A highly sensitive isotope dilution-gas chromatography-tandem mass spectrometry (ID-GC-MS/MS) method combined with gel permeation chromatography (GPC) and solid-phase extraction (SPE) was developed. Calibration curves showed good linearity for all PAHs (R ^2?>?0.999), and the limit of quantification (LOQ) ranged from 0.42 to 2.7?µg?kg^?1. Average recoveries for these compounds were in the range of 52.5–117%, 52.6–119% and 81.4–108% at the concentrations of 10, 50 and 250?µg?kg^?1 with RSD of 1.8–15%, 0.9–15% and 1.0–15%, respectively. The proposed method was used for the analysis of nine Chinese medicinal herbs. Total levels of PAHs varied from 98.2?µg?kg^?1 (cassia seed) to 2245?µg?kg^?1 (eucommia bark). The highest level was found for phenanthrene (Phe) in liquorice root (631.3?µg?kg^?1), indigowoad leaf (551.0?µg?kg^?1), rose flower (435.2?µg?kg^?1) and eucommia bark (432.3?µg?kg^?1). The proposed method could provide a useful basis for safety monitoring of herbs and risk management for PAHs in the health food industry.     

Survey of the anticoccidial feed additive nicarbazin (as dinitrocarbanilide residues) in poultry and eggs

A survey was carried out on the occurrence of dinitrocarbanilide (DNC), the marker residue for nicarbazin, in poultry produced in Ireland during 2002–2004. Liver (n?=?736) and breast muscle samples (n?=?342) were tested. DNC residues were found in 40 and 26% of liver and breast muscle samples at levels greater than 12.5 and 5?µg?kg^?1, respectively. DNC residues were found at >200?µg?kg^?1 in 12 and 0% of liver and muscle samples, respectively. Samples of breast muscle (n?=?217) imported from 11 countries were also tested for DNC residues. A lower incidence of DNC residues (6%) was found in imported breast muscle. Egg samples (n?=?546) were tested and DNC residues were found in nine samples, with levels ranging between 14 and 122?µg?kg^?1. Analysis of poultry, carried out as part of official food inspection in the period 2004–2006, indicated a reduction in the number of broiler liver samples containing DNC at >200?µg?kg^?1, to approximately 7%. Low levels of DNC residues continue to be found in <2% of egg samples.     

Comparative study of three screening tests,two microbiological tube tests,and a multi-sulphonamide ELISA kit for the detection of antimicrobial and sulphonamide residues in eggs

The screening of antimicrobial residues in eggs is an especially important subject. Three different commercial kits for the screening of sulphonamides and other antimicrobials in eggs were validated in accordance with Decision 2002/657/EC: one enzyme-linked immunoabsorbant assay (ELISA) kit multi-sulphonamides (from RAISIO Diagnostics) and two microbiological tests (a Premi® test from DSM and an Explorer® kit from Zeu-Inmunotec). The false-positive rates were lower than 2% for all kits. The detection capabilities (CCβ) have to be as low as possible for banned substances and lower than the maximum residue limit (MRL) when MRLs have been set. The sensitivity of the Premi® test was better than that of the Explorer® test, probably because of the dilution of the eggs before the Explorer® test was used. The CCβ values towards most of the tested sulphonamides were satisfactory with the Premi® test (≤ 100 µg kg^?1). Performance in a proficiency test for the detection of sulphonamides in eggs with the Premi® test confirmed these results. The detection capabilities of tetracycline and doxycycline were at the level of the MRL or twice the MRL maximum. The detection capabilities for chlortetracycline and oxytetracycline were higher (four to six times the MRL). The detection capabilities for amoxicillin, neomycin, tylosin and erythromycin were lower than their respective MRLs. Detection capabilities for sulphonamides were much lower for the ELISA kit than for microbiological tests. The ELISA kit could be recommended for the targeted screening of sulphonamides in eggs. On the other hand, the Explorer® and Premi® tests could be used as wide screening tests allowing the detection of most of the antimicrobial families.     

Determination of acrylamide in Thai-conventional snacks from Nong Mon market,Chonburi using GC-MS technique

Acrylamide in Thai-conventional snacks was analysed by GC/MS with a linear response ranged of 5–50?µg and r ^2?>?0.99. The limit of detection (s/n?=?(3) and limit of quantification (s/n?=?10) were 4 and 15?µg?kg^?1, respectively, and RSD?<?2%. Acrylamide in 19 food samples ranged from <15?µg?kg^?1 to 1.26?mg?kg^?1 with highest concentrations in Kanom Jak. Moderate levels (150–500?µg?kg^?1) were detected mostly in deep-fried products, especially sweet potato and taro crisps, Kanom Kai Hong, banana fritters, durian chips and spring rolls. Thai-conventional snacks possessed low concentrations (<150?µg?kg^?1) including Khao Larm, Pa Tong Koo, sweet banana crisps and deep-fried Chinese wonton. Acrylamide was lowest (<15?µg?kg^?1) in fish strips, rice crackers, Hoi Jor and fried fish balls. Dietary habits by 400 tourists indicate a daily intake of acrylamide <150?ng, well below a toxic dose.     

In-house validation of an ELISA method for screening of semicarbazide in eggs

An enzyme-linked immunosorbent assay (ELISA) method is described for the semi-quantitative determination of semicarbazide (SEM), the marker residue for the banned nitrofuran drug, nitrofurazone, in chicken eggs. The sample homogenate is subjected to acid hydrolysis and derivatisation with o-nitrobenzaldehyde, followed by ethyl acetate/hexane extraction and detection by ELISA. The ELISA procedure has been validated using 0.3, 1.0 and 3 µg kg^?1 of SEM in fortified samples. Detection capability (CC_ß) was based on the acceptance of 5% false compliant results for a given concentration level according to Commission Decision 2002/657/EC and was determined to be 0.3 µg kg^?1 with a respective limit of detection of 0.13 µg kg^?1. A validated LC–MS/MS method was used for the analysis of incurred egg samples and the results compared with ELISA. A good correlation between the results obtained from ELISA and LC–MS/MS within the concentration range 0.12–20.3 µg kg^?1 was observed in samples collected from chickens fed with a medicated ration of nitrofurazone (r?=?0.992, n?=?14). Validated ELISA enabled reliable monitoring of SEM levels in eggs collected from incurred chickens over a 90-day period.     

Evaluation of three different microbial inhibition tests for the detection of sulphamethazine residues in the edible tissues of rabbit

The aim of the present study was to evaluate three microbial inhibition tests (MIT) based on inhibition of growth of the test organisms: (a) four plate test (FPT) containing Bacillus subtilis BGA, (b) screening test for antibiotic residues (STAR) containing Bacillus stearothermophilus var. calidolactis_ATCC 10149 and (c) the Premi®Test containing Bacillus stearothermophilus var. calidolactis. The tests were used to determine sulphamethazine (SMZ) residues in edible tissues of rabbit after oral administration up to day 15 of the withdrawal period (WP). A solvent extraction procedure was used to enhance the capability of the tests to detect SMZ residues at or below the maximum residue limit (MRL). Para-aminobenzoic acid (PABA) was employed to previously identify SMZ residues in the first stage of the residue screening. The presence of SMZ residues in the samples was confirmed and quantified by a validated HPLC method. The Premi®Test detected SMZ residues in the muscle and heart tissue up to day 9 of the WP, and in the liver, lungs and kidneys up to day 10 of the WP. The STAR detected SMZ residues in the edible organs of rabbits up to day 8 of the WP. The kidneys were positive up to day 5 of the WP, the liver until day 4 of the WP and the lungs until day 3 of the WP. No SMZ residues were detected in the muscle and heart. By using the solvent extraction procedure, SMZ residues were detected in the muscle extract up to day 10 of the WP and the muscle was positive until day 6 of the WP. No detection sensitivity was observed using the FPT. After solvent extraction, SMZ residues were detected in the muscle extract until day 8 of the WP and the muscle was positive until day 3 of the WP. No positive results were detected after the addition of PABA into/onto the agar medium. PABA at a concentration of 10 µg ml^?1 completely reversed the inhibitory activity of SMZ and enabled reliable identification of SMZ in the examined samples. Using HPLC, SMZ was detected in the muscle samples until day 10 of WP (0.02 mg kg^?1) and in the liver until day 12 of the WP (0.09 mg kg^?1). The results obtained by the HPLC method and the limit of detection (LOD) of screening tests for SMZ (FPT 0.4 µg ml^?1, STAR 0.2 µg ml^?1, Premi® Test 0.05 µg ml^?1) allowed us to state that the most suitable screening tests for the detection of SMZ residues in the edible tissues of rabbits at level corresponding to the MRL of 0.1 mg kg^?1, established for sulphonamides, are the Premi®Test and STAR in conjunction with the solvent-extraction procedure.     

Immunoaffinity chromatography purification and ultra-high-performance liquid chromatography-tandem mass spectrometry determination of four β-agonists in beef

A highly selective and sensitive method was developed for the simultaneous determination of four β-agonists (clenbuterol, salbutamol, ractopamine and terbutaline) in beef by immunoaffinity chromatography purification coupled to ultra-high-performance LC-MS/MS. The MS/MS conditions, ultra-high-performance LC mobile phase, injection solution, sample purification process and matrix effect were studied to optimise the operation conditions. The limits of detection (LODs) of the instrument for the studied β-agonists ranged from 0.20 to 0.25?µg?l^?1, and the LODs of the method for the studied β-agonists ranged from 0.20 to 3.00?µg?kg^?1 for beef. Calibration curves were constructed using a standard solution diluted with blank beef matrix. The linear ranges of the calibration curves ranged from 5 to 100?µg?kg^?1 and the coefficients of determination were >0.9942 (n?=?10) for all four β-agonists. Samples spiked at 5, 10 and 50?µg?kg^?1 showed recoveries >72% and RSDs <6.6%. The method is suitable for the simultaneous detection of four β-agonists at trace levels in beef.     

Mass spectrometric analysis of muscle samples to detect potential antibiotic growth promoter misuse in broiler chickens

Mass spectrometric methods were developed and validated for the analysis in chicken muscle of a range of antibiotic growth promoters: spiramycin, tylosin, virginiamycin and bacitracin, and separately for two marker metabolites of carbadox (quinoxaline-2-carboxylic acid and 1,4-bisdesoxycarbadox), and a marker metabolite of olaquindox (3-methyl-quinoxaline-2-carboxylic acid). The use of these compounds as antibiotic growth promoters has been banned by the European Commission. This study aimed to develop methods to detect their residues in muscle samples as a means of checking for the use of these drugs during the rearing of broiler chickens. When fed growth-promoting doses for 6 days, spiramycin (31.4?µg?kg^?1), tylosin (1.0?µg?kg^?1), QCA (6.5?µg?kg^?1), DCBX (71.2?µg?kg^?1) and MQCA (0.2?µg?kg^?1) could be detected in the muscle 0 days after the withdrawal of fortified feed. Only spiramycin could consistently be detected beyond a withdrawal period of 1?day. All analytes showed stability to a commercial cooking process, therefore raw or cooked muscle could be used for monitoring purposes.     

Identification and quantification of the migration of chemicals from plastic baby bottles used as substitutes for polycarbonate

The results of a study on the analytical identification and quantification of migration of chemicals from plastics baby bottles found in the European Union market made of materials that are now present as substitutes for polycarbonate (PC) are reported. A total of 449 baby bottles with a focus on first age or sets of bottles were purchased from 26 European Union countries, Canada, Switzerland and the USA. From this collection, which contained several duplicates, a total of 277 baby bottles were analysed. The materials included different types of plastic such as PC, polyamide (PA), polyethersulphone (PES), polypropylene (PP), but also silicone, and from the United States a co-polyester marketed under the trade name Tritan?. The bottles were subjected to the conventional migration test for hot fill conditions, i.e. 2?h at 70°C. The simulant used was that specified in European Union legislation (2007/19/EC) for milk, i.e. 50% ethanol. In a first phase 1, migration was conducted since the scope of this investigation was a screening rather than a true compliance testing check. Second and third migrations were performed on selected articles when migrated substances exceeded limits specified in the legislation. In order to verify some materials, a portion of the bottle was cut to run an FT-IR fingerprint to confirm the nature of the polymer. The migration solutions in general showed a low release of substances. Results showed that bottles made of PP and silicones showed a greater number of substances in the migration solutions and in greater quantity. Chemicals from PP included alkanes, which could be found in >65% of the bottles at levels up to 3500?µg?kg^?1; and benzene derivatives in 17% of the baby bottles and found at levels up to 113?µg?kg^?1. Some substances were found on a regular basis such as plasticisers, esters and antioxidants (e.g. tris(2,4-di-tert-butylphenyl)phosphate, known as Irgafos 168. Some substances found were not included in the Community positive list, which means that those should not be found even in the first migration. Such substances included 2,6-di-isopropylnaphthalene (DIPN), found in 4% of the bottles at levels up to 25?µg?kg^?1, 2,4-di-tert-butyl phenol (in 90% of the bottles at levels up 400?µg?kg^?1). Moreover, bisphenol A (BPA) was detected and quantified in baby bottles made of PA, but limited to one brand and model specific (but labelled BPA free). Results for baby bottles made of silicone also indicated the presence of components, e.g. potentially coming from inks (benzophenone, diisopropyl naphtahalene – DIPN, which could come for example from the presence of instruction leaflets in the bottles). In the case of silicone, phthalates were also found in relevant concentrations, with levels for DiBP and DBP from the first migration test of 50–150?µg?kg^?1 and DEHP at levels 25–50?µg?kg^?1.     

Feed additives diclazuril and nicarbazin in egg and liver samples from Croatian farms

In total 307 egg and 275 liver samples were examined for nicarbazin and 365 eggs for diclazuril over a 30-month period. Enzyme-linked immunosorbent assay methods used for quantification were validated according to European Commission Decision 2002/657/EC. Non-compliant samples were confirmed by LC-MS/MS. Mean diclazuril concentrations in egg samples were 0.31?µg?kg^?1, which is below the MRL. In only one egg sample, 2.26?µg?kg^?1 was determined by enzyme-linked immunosorbent assay, although confirmation by LC-MS/MS gave a value of 1.6?µg?kg^?1. Mean nicarbazin levels determined were 1.85?µg?kg^?1 in egg and 21.1?µg?kg^?1 in liver samples. Four samples, one egg and three livers, yielded elevated concentrations of nicarbazin, but only in the egg sample the LC-MS/MS method confirmed nicarbazin (106?µg?kg^?1) above the MRL value.     

Simultaneous determination of type A,B and D trichothecenes and their occurrence in cereals and cereal products

A sensitive LC–MS/MS method for the simultaneous determination of type A, B and D trichothecenes in cereals is presented. The limits of detection ranged between 0.1 and 0.7 µg kg^?1 for all analytes. The method was applied to 289 representatively drawn samples of wheat, rye and oat products. Ninety-four percent of the wheat samples (n = 130), 95% of the rye samples (n = 61) and 100% of the oat samples (n = 98) were contaminated with the type A trichothecenes T-2 and HT-2 toxin. Median levels of T-2/HT-2 (sum of the toxins) were 0.91, 0.53 and 8.2 µg kg^?1, respectively. Highest levels were found in wheat bran (24 µg kg^?1), rye kernels (3.1 µg kg^?1) and oat flakes (85 µg kg^?1). All wheat and rye samples and 75% of the oat samples were contaminated with the type B trichothecene deoxynivalenol. Median levels of this toxin were 23, 15 and 0.53 µg kg^?1, respectively. Highest levels were found in wheat bran (1160 µg kg^?1), rye kernels (288 µg kg^?1) and oat flakes (55 µg kg^?1). The type B trichothecene nivalenol was detected in 67% of the wheat samples, in 3% of the rye samples and in 24% of the oat samples with highest levels in wheat bran (96 µg kg^?1), rye kernels (1.8 µg kg^?1) and in oat flakes (17 µg kg^?1), respectively. Levels of other type A and B trichothecenes played a minor role, although the rates of contamination were often high. Neither macrocyclic type D trichothecenes (satratoxin G and H, verrucarin A, roridin A) nor diacetylverrucarol and verrucarol (type A trichothecenes), were detected in any of the samples.     

Survey of aflatoxins in chillies from Pakistan produced in rural,semi-rural and urban environments

Chilli peppers from Pakistan are consumed locally and also exported. Their quality is compromised by aflatoxins (AF) contamination. AF in chillies from rural, semi-rural and urban areas of the Punjab region of Pakistan were determined. Twenty-three (52.3%), 22 (50%) and 29 (65.9%) samples from rural, semi-rural and urban areas respectively, contained levels of aflatoxins which exceeded the European Union limits of >5?µg?kg^?1 for AFB₁ and >10?µg?kg^?1 for total AF that apply to spices. Mean values for AFB₁ in ground samples were 23.8, 14.8 and 14.0?µg?kg^?1 for rural, semi-rural and urban areas, respectively. Mean total AF in ground samples were 27.7, 17.7 and 16.2?µg?kg^?1 from equivalent locations. Eleven (50%), 12 (54.5%) and 14 (63.6%) whole samples from rural, semi-rural and urban areas, respectively, contained total levels of AF that exceeded European Union limits. The data indicate that individual localities have particular problems. In conclusion, the concentrations were often greater than the statutory limits set by the European Union.     

Occurrence of furan in commercial processed foods in Brazil

Selected commercial processed foods available in the Brazilian market (306 samples) were analysed for furan content using a validated gas chromatography-mass spectrometry method preceded by headspace solid phase micro-extraction (HS-SPME-GC/MS). Canned and jarred foods, including vegetable, meat, fruit and sweet products, showed levels up to 32.8?µg?kg^?1, with the highest concentrations observed in vegetables and meats. For coffee, furan content ranged from 253.0 to 5021.4?µg?kg^?1 in the roasted ground coffee and from not detected to 156.6?µg?kg^?1 in the beverage. For sauces, levels up to 138.1?µg?kg^?1 were found. In cereal-based products, the highest concentrations (up to 191.3?µg?kg^?1) were observed in breakfast cereal (corn flakes), cracker (cream crackers) and biscuit (wafer). In general, these results are comparable with those reported in other countries and will be useful for a preliminary estimate of the furan dietary intake in Brazil.     

Aflatoxin M1 contamination in cow and buffalo milk samples from the North West Frontier Province (NWFP) and Punjab provinces of Pakistan

A total of 178 milk samples (94 of buffalo and 84 of cow) were randomly taken from Punjab and the North West Frontier Province (NWFP) of Pakistan (n?=?89 in each province) and analysed for the presence of aflatoxin M1 (AFM₁) by HPLC-FLD. From Punjab about 46% of buffalo's and 49% of cow's milks were contaminated with AFM₁ as compared with 52% and 51% for milk samples from NWFP, respectively. Overall, the mean AFM₁ concentration was 0.046?µg?kg^?1 with a maximum of 0.350?µg?kg^?1. All samples complied with the Codex Alimentarius limit of 0.50?µg?kg^?1 for AFM₁ in milk, but 16.3% of samples exceeded the European Union maximum level of 0.05?µg?kg^?1. Another set of 415 buffalo's and cow's milk samples (213 morning milks and 202 evening milks) were analysed. Statistical analysis revealed significant differences (p?<?0.05) between mean AFM₁ concentrations in milk during the morning (0.043?µg?kg^?1) and the evening (0.028?µg?kg^?1) lactation times.