Detection of ochratoxin A in tropical wine and grape juice from Brazil

BACKGROUND: Ochratoxin A (OTA) is the main mycotoxin found in grapes, wines and grape juices and is considered one of the most harmful contaminants to human health. In this study, samples of tropical wines and grape juices from different grape varieties grown in Brazil were analysed for their OTA content by high‐performance liquid chromatography. RESULTS: The detection and quantification limits for OTA were 0.01 and 0.03 µg L^?1 respectively. OTA was detected in 13 (38.24%) of the samples analysed, with concentrations ranging from < 0.03 to 0.62 µg L^?1. OTA was not detected in any of the grape juice samples. Most of the red wine samples proved to be contaminated with OTA (75%), while only one white wine sample was contaminated. However, the OTA levels detected in all samples were well below the maximum tolerable limit (2 µg L^?1) in wine and grape juice established by the European Community and Brazilian legislature. CONCLUSION: The results of this study indicate a low risk of exposure to OTA by consumption of tropical wines and grape juices from Brazil. © 2012 Society of Chemical Industry     

Voltammetric analysis of DL‐α‐tocopherol with a paste electrode

BACKGROUND: A voltammetric study of vitamin E (DL‐ α‐tocopherol) detection using square wave stripping and cyclic voltammetry is discussed in this paper. The working sensor was made by mixing carbon nanotube powder with DNA (double‐stranded calf thymus DNA) and mineral oil. In this electrode, the anodic peak was obtained for ? 0.6 V in a 0.1 mol L^?1 phosphate electrolyte solution. RESULTS: Under optimized stripping conditions, analytical linear working ranges of 0.5–4.0 µg L^?1 and 40.0–160.0 µg L^?1 were obtained. The RSD precision was pegged at 0.105% with seven points using an 80 µg L^?1 spike. The detection limit (S/N) was found to be 0.056 µg L^?1 (1.30 × 10^?10 mol L^?1). CONCLUSION: The developed method was found to be applicable to quality control analysis in the food, pharmaceutical and other manufacturing sectors. Copyright © 2008 Society of Chemical Industry     

Quantitative analysis of patulin in apple juice by thin-layer chromatography using a charge coupled device detector

A method was developed and validated in-house for the detection and quantification of patulin in apple juice concentrate using a charge coupled device (CCD) on thin-layer chromatography (TLC) plates. Samples were extracted with ethyl acetate and then cleaned-up by extraction with a sodium carbonate solution. The method showed a mean recovery of 95%. The quantification and detection limit were 14 µg l^?1 and 0.005 µg per spot, respectively. The CCD camera is sufficiently sensitive to detect changes in spot fluorescence intensity caused by small differences in mycotoxin concentration under homogeneous illumination from a UV light source. The results of validation confirmed the efficiency of the method, which is sensitive enough to be used to quantify patulin in apple juice by producers or for government monitoring/survey programs. The method was applied to the analysis of 16 apple juice concentrate samples and patulin levels ranged from 15 to 46 µg l^?1. This study demonstrated the applicability of the TLC–CCD technique as a tool for monitoring patulin in apple juice.     

Quantification of four arsenic species in fruit juices by ion-chromatography–inductively coupled plasma–mass spectrometry

A method using ion chromatography–inductively coupled plasma–mass spectrometry (IC–ICP–MS) for the quantification of arsenic species in fruit juices has been developed and validated. The method is capable of quantifying four anionic arsenic species – arsenite (As(III)), arsenate (As(V)), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) – in the presence of unretained species such as arsenobetaine (AsB). Method validation was based on repeatability, analysis of reference materials, recovery of fortified samples, and determination of detection and quantification limits. The method was tested for use with apple, pear, cranberry, grape (red, white and purple) juices, as well as several juice blends. Limits of detection were 0.35, 0.41, 0.45 and 0.70?µg?kg^?1 for As(III), DMA, MMA and As(V), respectively. Chromatographic recovery was good for most samples (90–107% compared to total arsenic), though recovery for some grape juice samples was lower (67–78%).     

Ochratoxin A in wines,musts and grape juices from Spain

A survey on the occurrence of ochratoxin A (OTA) in 240 grape‐based beverages was carried out. Red and white wines from four different Spanish Designations of Origin (n = 160), musts (n = 20), grape juices (n = 10), ordinary wines (n = 20), special wines (Malaga, muscatel, sherry, vermouth, etc) (n = 20) and sparkling wines (n = 10) were assayed for OTA content using immunoaffinity column clean‐up and high‐performance liquid chromatography with fluorimetric detection (detection limit 0.05 µg l^?1). Forty‐three (17.9%) of the samples tested contained detectable levels of OTA. The overall mean OTA concentration in red and white wines of Designations of Origin was 0.30 and 0.18 µg l^?1 respectively (ranges 0.05–3.19 and 0.05–1.13 µg l^?1 respectively). The percentage of wine samples with detectable amounts of OTA was higher for red (18.3%) than for white (10%) wines. OTA was also found in two of 10 red ordinary wines (0.68 and 4.24 µg l^?1), whereas none of 10 white ordinary wines contained OTA. The mean OTA amount detected in sparkling wines was 0.44 µg l^?1 (range 0.14–0.71 µg l^?1). Two of 20 must samples contained OTA at low levels (0.08 and 0.18 µg l^?1), while none of 10 grape juice samples contained OTA. Highest amounts of OTA were found in special wines (45%), with a maximum of 15.25 µg l^?1 in a muscatel sample. Copyright © 2004 Society of Chemical Industry     

Isolation of eriocitrin (eriodictyol 7‐O‐rutinoside) as an arachidonate lipoxygenase inhibitor from Lumie fruit (Citrus lumia) and its distribution in Citrus species

An inhibitory compound acting against rat platelet 12‐lipoxygenase was isolated from the peel of Lumie fruit (Citrus lumia) by activity‐guided separation. It was identified as eriocitrin (eriodictyol 7‐O‐rutinoside) by spectroscopic analyses. Eriocitrin inhibited 5‐lipoxygenase (IC₅₀29.1 µmol L^?1) from rat peritoneal polymorphonuclear leukocytes in addition to 12‐lipoxygenase (IC₅₀22.3 µmol L^?1). Its aglycone, eriodictyol (5,7,3′, 4′‐tetrahydroxyflavanone), was a much more potent inhibitor of both 12‐lipoxygenase (IC₅₀0.07 µmol L^?1) and 5‐lipoxygenase (IC₅₀0.20 µmol L^?1). It also inhibited the production of leukotriene B₄ in intact peritoneal polymorphonuclear leukocytes stimulated with calcium ionophore A23187 (IC₅₀12.7 µmol L^?1). The distribution of eriocitrin in 39 citrus fruits was investigated by high‐performance liquid chromatography analysis. Lumie, eureka lemon (Citrus limon), Sambokan (Citrus sulcata), Sudachi (Citrus sudachi) and Koji (Citrus leiocarpa) fruits were found to contain high levels of eriocitrin in both peel and juice vesicles. Copyright © 2006 Society of Chemical Industry     

Rapid determination of ethyl carbamate in Chinese rice wine using headspace solid‐phase microextraction and gas chromatography–mass spectrometry

Ethyl carbamate (EC) is a naturally occurring toxic contaminant that may imply a risk to human health and is usually found in alcoholic beverages such as Chinese rice wine. An automated procedure for the rapid determination of EC in Chinese rice wine was developed by headspace solid‐phase microextraction (HS‐SPME) coupled to gas chromatography–mass spectrometry (GC‐MS). Using propyl carbamate as internal standard, the optimized HS‐SPME sampling with a polyacrylic fibre was 45 min at 70°C after applying 38.8% NaCl to saturate the sample. This method showed good linearity over a range of 25–600 µg L^?1 (R² = 0.997). The recovery, relative standard deviation and limit of detection were 90.21–97.35%, lower than 2.89% and 1.19 µg L^?1, respectively. Additionally, the ethanol concentration had no effect on the analysis of EC. The total analysis time of 57 min per sample in continuous determination was twice as fast as the widely used solid‐phase extraction–GC‐MS method. This solvent‐free HS‐SPME‐GC‐MS procedure is suitable for the rapid, automated, and therefore convenient, determination of EC in Chinese rice wine. Copyright © 2012 The Institute of Brewing & Distilling     

Determination of melamine in milk powder,milk and fish feed by capillary electrophoresis: a good alternative to HPLC

BACKGROUND: Since September 2008, an increased incidence of kidney stones and renal failure in infants, associated with the ingestion of infant formula contaminated with melamine has been reported in China. Furthermore, melamine was not only found in many protein‐based food commodities, but also in the feeds for cattle and poultry. So it is necessary to develop a suitable method to determine melamine. RESULTS: A capillary zone electrophoresis (CZE) method for analysis of melamine was developed by use of running electrolyte containing 35 mmol L^?1 sodium dihydrogen phosphate at pH 3.5, with UV detection at 210 nm. Regression equation revealed linear relationships (r = 0.9999) between the peak‐area and the content of melamine from 0.8 to 80 µg mL^?1. The detection limit was 0.08 µg mL^?1. The method was successfully applied to the determination of melamine in milk powder, milk and fish feed, with the recoveries from 94.5% to 103.7%. CONCLUSION: The performance of the CZE method evaluated in terms of precision, limits of detection, accuracy and quantification were comparable and in good agreement with those obtained by the HPLC method, with the advantage of shorter analysis time and lower cost. Copyright © 2010 Society of Chemical Industry     

A sensitivity-improved enzyme-linked immunosorbent assay for fenvalerate: a new approach for hapten synthesis and application to tea samples

BACKGROUND: Fenvalerate has been widely used for the control of many common pests, but residues of this pesticide have been found in some agricultural crops. China is a large exporter of tea products; thus monitoring of pesticide residues in tea products has become increasingly important. In this study, a method of competitive direct enzyme‐linked immunosorbent assay (CD‐ELISA) for the rapid detection of fenvalerate in tea sample was developed. RESULTS: A polyclonal antibody against fenvalerate (FEN) was produced by the hapten with the characteristic moiety of fenvalerate. After acidification, the hapten was synthesized from 2‐(4‐chloro‐phenyl)‐3‐methyl‐butyric acid and aminocaproic acid methyl ester. The CD‐ELISA method developed has a high sensitivity of detection: 9 µg L^?1 for IC₅₀ and 0.5 µg L^?1 for IC₁₅. Fenvalerate was treated with 0.5 mmol L^?1 NaOH–methanol solution to improve its solubility by isomerization. In the tea sample, the detection limit of fenvalerate was 0.16 mg L^?1. A recovery rate of 76.67–91.43% was obtained from spiked tea. The reliability of the CD‐ELISA method is better in comparison with the gas chromatographic method (R² = 0.9968). CONCLUSION: In this study, a simple and efficient immunoassay method was developed. It is preferable for the rapid determination of fenvalerate residues in tea samples. Copyright © 2011 Society of Chemical Industry     

Natural deep eutectic solvent-based ultrasound-assisted-microextraction for extraction,pre-concentration and analysis of methylmercury and total mercury in fish and environmental waters by spectrophotometry

ABSTRACT

In this study, a simple, pH-controlled, and natural deep eutectic solvent-based microextraction (NADES-ME) procedure is proposed before the spectrophotometric analysis of methylmercury (MeHg) and total mercury in fish and environmental waters. The method is based on charge-transfer sensitive ion-pair formation between MeHg and 3-(dimethylamino)-7-(methylamino)phenothiazin-5-ium chloride (Azure B – AzB) in the presence of chelating citrate-phosphate buffer at pH 6.0, and then extraction of the formed ion-pair complex with the NADES. The important variables affecting extraction efficiency were evaluated and optimised. At optimal conditions (300 µL of 1.0 × 10^?3 mol L^?1 AzB, 600 µL NADES (betaine-sorbitol, 1:3) containing 10% water (v/v) as extractant, 375 µL acetonitrile as aprotic solvent for sonication of 7 min at power of 300 W/40 kHz, and centrifugation at 4000 rpm for 3 min, respectively), the figures of merit for MeHg include a good linearity in the concentration range of 0.7–340 µg L^?1, limits of detection and quantification of 0.25 and 0.83 µg L^?1, and pre-concentration and sensitivity enhancement factors of 120 and 95, respectively. Figures of merit for total Hg (iHg, where Hg₂²⁺ ions are predominantly present in natural oxygen-rich waters such as freshwaters and seawater as well as elemental Hg and Hg²⁺ ions at very low amounts) after pre-oxidation at pH 5.0 include linearity range of 3–270 µg L^?1 with limits of detection and quantification of 0.92 and 3.10 µg L^?1, and pre-concentration and sensitivity enhancement factors of 120 and 35, respectively. The reliability (with recovery of 92–98.7% and RSD of 1.9–5.5%) was statistically validated by analysis of two standard reference materials (SRMs) with and without spiking. The method was successfully applied to the speciation analysis of total Hg, iHg and MeHg in fish and environmental waters.     

A novel common single primer multiplex polymerase chain reaction (CSP‐M‐PCR) method for the identification of animal species in minced meat

BACKGROUND: Minced meat species adulteration is a severe problem. In this study a common single primer multiplex polymerase chain reaction (CSP‐M‐PCR) method was applied to the identification of five species (chicken, cattle, sheep, pig and horse) in minced meat products. CSP was designed as a common adapter at the 5′‐end of species‐specific reverse primers and employed in giving different length fragments from the respective meat species. RESULTS: Species‐specific DNA fragments could be identified in a single PCR reaction by mixing CSP, Chicken‐R, Cattle‐R, Sheep‐R, Pig‐R and Horse‐R primers in the ratio 1:0.01:0.01:0.01:0.01:0.10 (where ‘1’ represents 0.5 mmol L^?1). The specific DNA fragments could be efficiently amplified by CSP‐M‐PCR with > 5 µmol L^?1 species‐specific primers, except for 50 µmol L^?1 Horse‐R. A detection limit of 0.5 g kg^?1 was determined for both single species of minced meat and all species of five kinds of minced meat. CONCLUSION: The CSP‐M‐PCR method simplified the PCR reaction system and removed the inconsistent amplification efficiency from different primers. This highly sensitive, reproducible and rapid method could potentially be used as a screening or identifying assay to test for the presence of species or ingredients in minced meat and other meat products. Copyright © 2008 Society of Chemical Industry     

Antioxidant activity and phenolic content of wine vinegars produced by two different techniques

BACKGROUND: The presence of phenolics in fruit, red wine and vinegar has positive health effects due to their significant antioxidant activity. The aim of the study was to determine the effects of two different vinegar production methods on antioxidant activity and phenolic level of vinegars derived from Ulugbey Karasi grapes. Traditional surface and industrial submerge methods were used to make vinegar. Samples were taken from fresh red grape juice, maceration, wine, traditional vinegar and industrial vinegar. RESULTS: Total phenolic content of traditional and industrial vinegar samples were 2690 mg L^?1 and 2461 mg L^?1 GAE, respectively. ORAC values of traditional and industrial vinegar samples were 10.50 µmol mL^?1and 8.84 µmol mL^?1 TE, respectively. Antioxidant activity values of traditional and industrial vinegars were 13.50 mmol L^?1 and 10.37 mmol L^?1 TEAC, respectively. Gallic acid, catechin, epicatechin, chlorogenic acid, caffeic acid, syringic acid, p‐coumaric acid and ferulic acid were detected in grape juice, wine and vinegar samples. The content of catechin in industrial vinegar (27.50 mg L^?1) was significantly higher than that of in traditional vinegar (13.76 mg L^?1) (P < 0.05). Traditional vinegar had higher amounts of chlorogenic and syringic acids than the industrial vinegar (P > 0.05). CONCLUSION: Results of this study showed that different production methods affected the functional constituents of wine vinegars. Copyright © 2010 Society of Chemical Industry     

Hydroxymethylfurfural in fruit puree and juice: preconcentration and determination using microextraction method coupled with high-performance liquid chromatography and optimization by Box–Behnken design

In the present study, a sensitive and rapid method for separation and determination of hydroxymethylfurfural (HMF) in fruit puree and juices was proposed. Dispersive liquid–liquid microextraction (DLLME) coupled with high-performance liquid chromatography (HPLC) was used for extraction and quantitative determination of HMF in fruit puree and juices. The effective parameters such as the type and volume of extraction and dispersive solvents, pH and salt amount (NaCl) were studied and optimized with the aid of response surface methodology based on Box–Behnken design to obtain the best condition for HMF extraction. At the optimized conditions, parameter values were 60 µL extracting solvent, 600 µL dispersive solvent, 2 g NaCl and pH 5. Repeatability of the method, described as the relative standard deviation, was 3.1% (n?=?6) and the recovery was 98.4%. The limit of detection and limit of quantitation were 1.47 and 5.28 µg L^?1, respectively. The merit figures of DLLME–HPLC–UV method showed that the proposed method can be noticed as a new, fast and good alternative method for investigation of HMF in various fruit puree and juice samples.     

Multitoxin extraction and detection of trichothecenes in cereals: an improved LC‐MS/MS approach

BACKGROUND: Many multiresidual methods to evaluate natural occurrence of Fusarium toxins are already reported in the scientific literature but a new rapid, reliable, cost‐efficient and high‐sensitivity method for the simultaneous determination of several fusariotoxins is always welcome. Nivalenol (NIV), deoxynivalenol, fusarenon‐X (FUS‐X), 3‐acetyldeoxynivalenol, diacetoxyscirpenol (DAS), HT‐2 toxin, T‐2 toxin, neosolaniol (NEO), zearalanone and zearalenone (ZON) belong to the most common mycotoxins in food matrix grains, e.g., wheat and maize. The proposed method is a multitoxin analytical method that combines high‐performance liquid chromatography (HPLC), atmospheric pressure chemical ionization (APCI), triple‐quadrupole tandem mass spectrometry (LC‐MS/MS) under the selected reaction monitoring (SRM) mode, and it is focused on the optimization of the sample preparation without the need for any cleanup. RESULTS: Three different methods for sample preparation and for the simultaneous extractions of the above‐mentioned fusariotoxins were tested: two of these were followed by a different cleanup step for comparison, while the extraction method proposed in this work, which uses an 84% (v/v) acetonitrile aqueous solution, sample homogenization and subsequent filtration, was validated without any further cleanup step. CONCLUSION: Calibration curves for all analytes are linear, except DAS, HT‐2 and ZON, over the working range of 10–1000 µg kg^?1. The calibration curve of DAS was linear between 10 and 500 µg kg^?1, although the curves of HT‐2 and ZON were linear in the range 10–250 µg kg^?1. Squared correlation coefficients (R²) were in the range 0.995–0.998 for the all point calibration curves. The lowest limits of detection (LOD) were found for DON and ZAN with 0.5 and 0.2 µg kg^?1, respectively, while the highest LODs were obtained for NIV, FUS‐X and NEO, with 3.3 µg kg^?1 for each toxin. Copyright © 2009 Society of Chemical Industry     

Juice components and antioxidant capacity of four Tunisian Citrus varieties

BACKGROUND: Juices from four Citrus species of Tunisia were investigated mainly for quality parameters and antioxidant capacity. RESULTS: Citrus reticulata (mandarin) juice had the highest content of total flavonoids (85.33 mg CE L^?1). The latter also occurred in high quantity (82.01 mg CE L^?1) in Citrus lemon (lemon) juice which was also marked by its richness in total aroma (70.16 µg mL^?1) and in total fatty acids (48.10 µg mL^?1). Mandarin and lemon juices had the highest antioxidant activity, as determined b the β‐carotene bleaching assay (26.67% and 22.67%, respectively). Citrus aurantium (bitter orange) juice was characterised by the highest content of total polyphenols (784.67 mg GAE L^?1) and by the greatest inhibition of DPPH (96.10%). Citrus sinensis (blood orange) juice was only marked by the high quantity of ascorbic acid (36.90 mg mL^?1). GC/MS analysis of juice aroma showed the predominance of limonene (48.85–69.59%) in mandarin and in bitter and blood oranges, but of camphene (89.05%) in lemon. GC analysis of juice fatty acids revealed their richness in oleic acid (23.13–39.52%). HPLC analysis of juice phenolics indicated the predominance of phenolic acids (73.13–86.40%). CONCLUSION: The Citrus species used in this study were considered valuable varieties from the point of view of antioxidant capacity and nutrition. Copyright © 2010 Society of Chemical Industry     

Carotenoids in yellow‐ and red‐fleshed papaya (Carica papaya L)

Vitamin A deficiency is a disorder of public health importance in Sri Lanka. A recent national survey revealed that 36% of preschool children in Sri Lanka have vitamin A deficiency (serum retinol <0.2 µg ml^?1). In view of its well‐established association with child morbidity and mortality, this is a reason for concern. One of the main fruits which has been recommended for prevention of vitamin A deficiency in Sri Lanka is papaya (Carica papaya L). In this study the carotenoid profiles of yellow‐ and red‐fleshed papaya were analysed by medium‐pressure liquid chromatography (MPLC) and UV‐vis spectrophotometry. A section of yellow‐fleshed papaya showed small carotenoid globules dispersed all over the cell, whereas in red‐fleshed papaya the carotenoids were accumulated in one large globule. The major carotenoids of yellow‐fleshed papaya were the provitamin A carotenoids β‐carotene (1.4 ± 0.4 µg g^?1 dry weight (DW)) and β‐cryptoxanthin (15.4 ± 3.3 µg g^?1 DW) and the non‐provitamin A carotenoid ζ‐carotene (15.1 ± 3.4 µg g^?1 DW), corresponding theoretically to 1516 ± 342 µg kg^?1 DW mean retinol equivalent (RE). Red‐fleshed papaya contained the provitamin A carotenoids β‐carotene (7.0 ± 0.7 µg g^?1 DW), β‐cryptoxanthin (16.9 ± 2.9 µg g^?1 DW) and β‐carotene‐5,6‐epoxide (2.9 ± 0.6 µg g^?1 DW), and the non‐provitamin A carotenoids lycopene (11.5 ± 1.8 µg g^?1 DW) and ζ‐carotene (9.9 ± 1.1 µg g^?1 DW), corresponding theoretically to 2815 ± 305 µg kg^?1 DW mean RE. Thus the carotenoid profile and organisation of carotenoids in the cell differ in the two varieties of papaya. This study demonstrates that carotenoids can be successfully separated, identified and quantified using the novel technique of MPLC. Copyright © 2003 Society of Chemical Industry     

Development of high‐performance liquid chromatography and non‐aqueous capillary electrophoresis methods for the determination of fenoxycarb residues in wheat samples

BACKGROUND: Practical methods for the analysis of fenoxycarb residues in wheat samples were developed using high‐performance liquid chromatography (HPLC) and non‐aqueous capillary electrophoresis (NACE). RESULTS: Fenoxycarb residues in wheat were extracted with acetone by ultrasonication, followed by a clean‐up procedure with liquid–liquid extraction with 5% NaCl/dichloromethane. The HPLC was developed using C18 as column, MeOH/water (6:4, v/v) as the mobile phase and 199 nm as the detection wavelength. The optimal NACE condition was established with the running buffer of 20.0 mmol L^?1 NH₄Ac in 95% MeOH (pH* 9.0), and the applied voltage of 30 kV over a capillary of 50 µm i.d. × 48.5 cm × 40 cm effective length. Both methods gave the relatively lower limits of detection (0.008 mg kg^?1 for HPLC and 0.024 mg kg^?1 for NACE) and the higher recoveries (>85.0%). They were successfully applied to the determination of fenoxycarb in wheat samples. CONCLUSION: The results showed that the fenoxycarb residue gradually reduced to trace amounts after about 3 years, which implied that the pharmacological actions of fenoxycarb could last for about 3 years. Meanwhile, more effort should be made to control and reduce fenoxycarb residues because of its potential health risks to consumers. Copyright © 2007 Society of Chemical Industry     

Multi-element determination in some foods and beverages using silica gel modified with 1-phenylthiosemicarbazide

ABSTRACT

1-Phenylthiosemicarbazide bonded modified silica gel (PTC-SG) was synthesised and characterised by FTIR, SEM and elemental analysis for a novel separation/preconcentration of multiple elements based on solid phase extraction. The analytical parameters including pH of solutions, amounts of PTC-SG, flow rates of sample, eluent type and sample volume were optimised. The adsorption capacities of PTC-SG were found to be 7.9, 6.4, 6.3, 8.3, 7.2, 8.9 and 6.6 mg/g for Cu(II), Cd(II), Pb(II), Co(II), Cr(III), Ni(II) and Mn(II), respectively. The limit of detection (LOD) was calculated as 3x the standard deviation(s) of the reagent blank (k = 3, N = 21) and the LOD values were obtained to be 0.98 µg L^?1 (Cu), 0.65 µg L^?1 (Cd), 0.57 µg L^?1 (Pb), 1.12 µg L^?1 (Co), 1.82 µL^?1 (Cr), 1.67 µg L^?1 (Ni) and 0.55 µg L^?1 (Mn). Certified reference materials were used to test the validation of the present method. The new solid phase extraction method was successfully applied to determination of the amount of multiple elements in food and beverage samples.     

Survey of aflatoxin M1 in cow's milk for human consumption in Kerman Province of Iran

The aim of this study was to assess levels of aflatoxin M₁ (AFM1) in milk samples from Kerman, Iran. AFM1 was detected in 72 samples, ranging in concentration from <0.01 to 0.41?µg?l^?1. The samples were analyzed using immunoaffinity column for clean-up and HPLC for determining AFM1. Milk samples were collected from six dairy farms. AFM1 was found in ～50% of the milk samples. The average level of AFM1 was below the tolerance limit (0.05?µg?l^?1), but 50% of the samples had greater levels than the maximum tolerance limit accepted by EU and the Iranian national standard. The method detection limit and limit of quantification were 0.01 and 0.03?µg?l^?1, respectively, and recovery of the method was 87%. The results showed that AFM1 contamination is a serious problem for public health. To achieve a low level of AFM1 in milk, cattle feed must be monitored regularly for aflatoxin contamination and protected from fungal contamination as much as possible.     

Validation of an HPLC Methodology for the Identification and Quantification of Biogenic Amines in Chicken Meat

This study validated a high performance liquid chromatography (HPLC) method to determine biogenic amines in chicken meat. For the identification of biogenic amines, an isocratic elution system coupled with a UV detector (254 nm) was used after a perchloric acid (5 %) extraction and benzoyl chloride derivatization of the samples. The standards of tyramine, putrescine, cadaverine, spermidine, and spermine were used for the following validation parameters: selectivity, linearity, accuracy, recovery, limit of detection and quantification, and robustness. Finally, chicken meat commercialized in two types of packaging was evaluated. The results showed an excellent selectivity and separation of all amines, r ²?>?0.99, relative standard deviation <5 %, recovery between 64 and 112 %, limits of detection and quantification between 0.03–1.25 and 0.15–5.00 μg?L^?1, respectively, and appropriate robustness for the proposed methodology. Moreover, both chicken meat commercial packages had similar values for all amines; only tyramine was significantly different (P?≤?0.05). The proposed method was suitable to detection and quantification of simultaneous five biogenic amines in chicken meat.