Stefania Albrizio

Determination of Bisphenol A and Bisphenol B Residues in Canned Peeled Tomatoes by Reversed-Phase Liquid Chromatography

Bisphenol A (BPA) and bisphenol B (BPB) concentrations were determined in peeled canned tomatoes of different brands bought in Italian supermarkets. Tomato samples analyzed were packaged in cans coated with either epoxyphenolic lacquer or low BADGE enamel. A solid phase extraction (SPE) was performed on C-18 Strata E cartridge followed by a step on Florisil cartridge. Detection and quantitation were performed by a reversed phase high-performance liquid chromatography (RP-HPLC) method with both UV and fluorescence detection (FD). On the total of 42 tested tomato samples, BPA was detected in 22 samples (52.4%), while BPB was detected in 9 samples (21.4%). BPA and BPB were simultaneously present in 8 of the analyzed samples. The levels of BPA found in this study are much lower than the European Union migration limits of 3 mg/kg food and reasonably unable to produce a daily intake exceeding the limit of 0.05 mg/kg body weight, established by European Food Safety Authority.

Occurrence of Fusarium mycotoxins and their dietary intake through beer consumption by the European population

Since cereals are raw materials for production of beer and beer-based drinks, the occurrence mycotoxins in 154 beer samples was topic of investigation in this study. The analyses were conducted using QuEChERS extraction and gas chromatography-tandem mass spectrometry determination. The analytical method showed recoveries for vast majority of analytes ranged from 70% to 110%, relative standard deviations lower than 15% and limits of detection from 0.05 to 8 μg/L. A significant incidence of HT-2 toxin and deoxynivalenol (DON) were found in 9.1% and 59.7% of total samples, respectively. The exposure of European population to mycotoxins through beer consumption was assessed. No toxicological concern was associated to mycotoxins exposure for average beer consumers. Despite that, for heavy beer drinkers, the contribution of this commodity to the daily intake is not negligible, approaching or even exceeding the safety levels.

Development and validation of a solid-phase extraction method coupled to high-performance liquid chromatography with ultraviolet-diode array detection for the determination of sulfonylurea herbicide residues in bovine milk samples

This study proposes a fast, simple and sensitive liquid chromatography diode array detector (LC/UV-DAD)-based method for the simultaneous determination of eight sulfonylurea herbicides (bensulfuron methyl, chlorsulfuron, metsulfuron methyl, primisulfuron methyl, rimsulfuron, thifensulfuron methyl, triasulfuron and tribenuron methyl) in bovine whole milk at concentrations lower than the default limit of 0.01 mg kg(-1) allowed by current legislation (Regulation EC/396/2005 and following Annexes). An effective one-step solid phase extraction (SPE) and clean up procedure was defined with use of Chem Elut cartridges, providing good recoveries for all the analytes tested and with no matrix effects affecting method accuracy. Separation of herbicides was obtained on a C(18) column by acetonitrile- water gradient elution. Method validation has been performed according to European Commission Decision 2002/657/EC criteria, in terms of linearity, recovery, precision, specificity, decision limit (CC(α)) and detection capability (CC(β)). Typical recoveries ranged between 78.4% and 99.7%, at the maximum residue limits (MRLs) levels established by Regulation EC/396/2005, with relative standard deviations (RSD) no larger than 10%.

A Simple and Selective Analytical Procedure for the Extraction and Quantification of Lutein from Tomato By-Products by HPLC–DAD

Lutein, a yellow dihydroxylated carotenoid, is present in many dietary supplements due to its biological properties. Currently, lutein is extracted from marigold flowers by expensive and time-consuming processes. Since tomatoes contain significant levels of lutein, in this study we have examined the feasibility of using tomato by-products as an alternative, low-cost source of this carotenoid. The determination of this carotenoid was performed by high-performance liquid chromatography–diode array detection, after selective extraction from tomato waste product samples. Lutein levels ranged from 9.9 to 10.5xa0μg/g dry weight. Tomato waste products may be indicated as an alternative commercial source of lutein for food fortification and/or dietary supplements.

Determination of five bisphenols in commercial milk samples by liquid chromatography coupled to fluorescence detection.

The presence of five bisphenols, i.e., bisphenol F, bisphenol A, bisphenol B, bisphenol F diglycidyl ether, and bisphenol A diglycidyl ether, was monitored in commercial milk packed in plastic bottles marketed in Italy. The new validated method includes a solid-phase extraction procedure followed by liquid chromatography with fluorescence detection. All positive results were confirmed by liquid chromatography-tandem mass spectrometry analysis. The limits of detection and quantification and the recovery percentages indicated that the method is suitable for detecting bisphenols in milk at concentrations far below the legal limits. Of 68 commercial milk samples analyzed, no bisphenol was found in 27 samples (39.7%), and 41 samples (60.3%) contained one or more bisphenols. The bisphenol most frequently found was bisphenol F (36 samples, 52.9%) followed by bisphenol A (20 samples, 29.4%) and bisphenol B (6 samples, 8.8%). Taking into consideration the limits of detection, no sample contained either bisphenol F diglycidyl ether or bisphenol A diglycidyl ether.

Monitoring of bisphenols in canned tuna from Italian markets.

Monitoring of food contamination from bisphenols is a necessary process for the consumers risk assessment. A method for the quali-quantitative analysis of Bisphenol A (BPA), Bisphenol B (BPB), Bisphenol A Diglycidyl Ether (BADGE), and Bisphenol F Diglycidyl Ether (BFDGE), by liquid chromatography with fluorescence detection (LC-FD), was performed and validated for their determination in 33 samples of tuna fish, canned in either oil or aqueous medium. Samples were collected in Italian markets. Tuna and the correspondent preservation medium were analyzed separately. Detected levels of bisphenols ranged from 19.1 to 187.0 ng/g in tuna matrix and from 6.3 to 66.9 ng/mL in oil medium. No bisphenols were found in aqueous medium. At least one of the analytes was found in 83% of the tuna samples in oil medium, whereas tuna samples in aqueous medium showed BPA alone in 67% of samples. 21% of the oil medium samples resulted positive for at least one bisphenol. On the basis of measured concentrations and general daily ingestion rate of canned tuna fish, the probable daily intake of BPA for Italian population was calculated.

Determination of dimethyl fumarate in desiccant and antimould sachets by reversed-phase liquid chromatography

A method for the determination of dimethyl fumarate (DMF) in desiccant and antimould sachets, employed for protecting consumer products from humidity and mould, has been developed. The method is based on a solid-liquid extraction followed by HPLC-UV analysis. The method was validated with respect to recovery, linearity, limits of detection and quantitation and precision. The recovery was 98%. The correlation coefficient value (r) was equal to 0.94. Both intra- and inter-day precisions were studied at several concentration levels, being satisfactory in all cases (RSDu2009<u20095). Limits of detection and quantification values were in the low microgram per gram level, thus allowing the determination of DMF at concentrations below the limit established (0.1u2009mg/kg) by the recent EU Directive (Decision 2009/251/EC). The proposed procedure was applied for the determination of the target compound in 41 desiccant and antimould samples. DMF was detected in 39.0% of samples and its content in many samples exceeded the legal limits. The results of our analysis highlight the high risk of exposure to this powerful allergic sensitizer for consumers.

A GC–FID Method to Determine Styrene in Polystyrene Glasses

The styrene levels of polystyrene (PS) glasses from the most consumed brands of disposable glasses intended for water and coffee in Brazil were determined. A GC–FID method was developed and validated, showing good precision and accuracy. The method was successfully used to determine styrene in 11 PS glass brands. The styrene levels ranged from 1.68 to 43.69xa0mg/100xa0g glass, depending on the kind of polymer, thickness, and glass brand. It could be used to control the content of styrene in the polymer. The migration of styrene from the glasses into water and 20xa0% ethanol was not detected.

A simple HPLC-DAD method for the analysis of melamine in protein supplements: validation using the accuracy profiles.

The study presents a fully validated simple high-performance liquid chromatography method with diode array detection (HPLC-DAD), able to accurately determine the melamine, fraudulently added, in protein supplements, commonly used from healthy adults to enhance exercise or sport performance. The validation strategy was intentionally oriented towards routine use and the reliability of the method rather than extreme performance. For this reason, validation by accuracy profile, including estimation of uncertainty, was chosen. This procedure, based on the concept of total error (biasu2009+u2009standard deviation), clearly showed that this method was able to determine melamine over the range of 0.05–3.0u2009mgu2009Kg−1, selected by taking into account the maximum residue levels (MRLs) proposed by European legislation to distinguish between the unavoidable background presence of melamine and unacceptable adulteration. The accuracy profile procedure established that at least 95% of the future results obtained with the proposed method would be within the ±15% acceptance limits of the validated HPLC-DAD method over the whole defined concentration range.

Development and validation of a diode array high performance liquid chromatography method to determine seized street cocaine sample purity

A novel, precise, specific, accurate and rapid reversed-phase high performance liquid chromatographic method, with diode array detection, was developed, optimized and validated to determine the drug purity of cocaine street samples seized in Italy and to characterize the adulterants. The method was performed using a C18 column, under isocratic conditions, with potassium phosphate buffer–acetonitrile as the mobile phase, at 232 nm. Linearity was studied from 0.01 to 0.50 mg mL−1, with a determination coefficient (r2) higher than 0.9999. The limit of detection (LOD) and limit of quantification (LOQ) were 0.004 mg mL−1 and 0.01 mg mL−1, respectively. Precision was evaluated as repeatability and intermediate precision with relative standard deviations not exceeding 5%. Validation of the HPLC method was carried out following ICH guidelines. Also, the estimation of the uncertainty measurements was included. The proposed HPLC-DAD method was thus shown to be convenient and highly suitable for the routine analysis of seized samples of drugs of abuse.