ABSTRACT In this study, heavy metal levels detected in molluscs produced in the Veneto Region (no... more ABSTRACT In this study, heavy metal levels detected in molluscs produced in the Veneto Region (north-western Adriatic Sea) are presented and discussed. A descriptive analysis was conducted on data collected in the framework of official monitoring activities in shellfish production areas between 2007 and 2012. Concentrations of lead (Pb), mercury (Hg) and cadmium (Cd) in about 2000 samples of 17 different species of marine bivalve molluscs, echinoderms and gastropods were checked by means of atomic absorption spectrometry. Hg and Pb concentrations were always below the maximum levels set by the European legislation; 2.2% of the analysed samples exceeded the threshold level for Cd, 86.7% of witch belonging to purple dye murex (Bolinus brandaris). The highest mean levels of Hg and Cd were found in purple dye murex, with 0.10 mg kg−1 and 0.88 mg kg−1 respectively, while rayed trough shell (Mactra stultorum) and truncate donax (Donax trunculus) were the species with the highest mean value of Pb (0.25 mg kg−1). Species of major consumption showed mean values almost ten times lower than the limits set by the European legislation (Manila clam: Pb: 0.20 mg kg−1; Hg: 0.04 mg kg−1; Cd: 0.07 mg kg−1; Mediterranean mussel: Pb: 0.22 mg kg−1; Hg: 0.03 mg kg−1; Cd: 0.13 mg kg−1). A preliminary evaluation of the impact on human health of shellfish according to the detected levels indicates that the species of major consumption are safe for the average consumers, although a potential risk cannot be ruled out for vulnerable groups, such as women of childbearing potential and children, as well as for regular or high-level shellfish consumers, particularly those who frequently eat species such as murex.
Honey, in particular monofloral varieties, is a valuable commodity. Here, we present proton trans... more Honey, in particular monofloral varieties, is a valuable commodity. Here, we present proton transfer reaction-time of flight-mass spectrometry, PTR-ToF-MS, coupled to chemometrics as a successful tool in the classification of monofloral honeys, which should serve in fraud protection against mispresentation of the floral origin of honey. We analyzed 7 different honey varieties from citrus, chestnut, sunflower, honeydew, robinia, rhododendron and linden tree, in total 70 different honey samples and a total of 206 measurements. Only subtle differences in the profiles of the volatile organic compounds (VOCs) in the headspace of the different honeys could be found. Nevertheless, it was possible to successfully apply 6 different classification methods with a total correct assignment of 81-99% in the internal validation sets. The most successful methods were stepwise linear discriminant analysis (LDA) and probabilistic neural network (PNN), giving total correct assignments in the external validation sets of 100 and 90%, respectively. Clearly, PTR-ToF-MS/chemometrics is a powerful tool in honey classification.
The applicability of gel permeation chromatography (GPC) to the purification in foodstuffs in the... more The applicability of gel permeation chromatography (GPC) to the purification in foodstuffs in the detection of three classes of drugs, sulfonamides, nitrofurans, and growth promoters, is described. This technique has already found a wide application in the routine analysis of pesticides in milk, eggs and grease but to our knowledge there is no published work on the use of GPC for purifying animal feedstuffs for the detection of the above-mentioned classes of drugs. Three main advantages characterize this method: the simultaneous determination of a wide spectrum of drugs; good performance of the purification system; and high recoveries. The method was tested for a determination limit of 1 ppm in each compound. Average recoveries of spiked samples were: 99% for sulfonamides; 98% for nitrofurans; and 100% for carbadox [methyl-3-(2-quinoxalinylmethylene) carbazate-1,4-dioxide] and olaquindox [N-(2-hydroxyethyl)-3-methyl-2-quinoxalinecarboxamide-1,4-dioxide] . The method was also tested for linearity over the range 1-100 ppm and gave r values between 0.9998 and 0.9999 for each drug. Analyses were performed by HPLC, either using a diode array or windowplot-system detector. The described method is quick and simple, which is very useful in routine analysis.
International Journal of Environmental Analytical Chemistry, 2015
ABSTRACT This work was performed to highlight the advantages of total reflection X-ray fluorescen... more ABSTRACT This work was performed to highlight the advantages of total reflection X-ray fluorescence spectroscopy (TXRF) for multi-elemental qualitative and quantitative analysis of wine. Indeed the International Organization of Vine and Wine (OIV) selected some potentially toxic elements and proposed limit values for their concentration in wines. Direct TXRF analysis of nine wine samples from Emilia Romagna region of Italy was performed in two different laboratories: Italy and Japan. Wine dehydration was also evaluated as sample conservation mean. Traces of Fe, Cu, Zn and Pb are present in all the analysed samples, with concentrations lower than the limits established by the OIV. The target hazard quotients (THQs) were also calculated for seven elements (Cl, Mn, Fe, Ni, Cu, Zn and Sr) to determine their potential detrimental effects. The results show that TXRF is a fast, simple and accurate analytical technique for trace element analysis of wine. Moreover, dehydration is an effective way to store wine samples for further elemental analysis.
A new chromatographic method is proposed for the analysis of aflatoxin M(1) in milk. The method i... more A new chromatographic method is proposed for the analysis of aflatoxin M(1) in milk. The method is based on liquid-liquid extraction followed by LC-MS/MS analysis. Liquid-liquid extraction (LLE) is performed on the defatted milk plus sodium chloride by using ethyl acetate as an extraction solvent. Accuracy and precision were evaluated at the LOQ (15 ng kg(-1)) spiked sample as well as with three other different naturally contaminated reference materials. The mean overall recovery (n = 24) was 95% with a confidence interval of 1.9% and a CV% of 4.5%. The performance of the proposed method was compared with that of the Official ISO Method based on the use of immunoaffinity chromatography columns (IAC): LLE protocol could be considered a valid alternative to the LC-IAC. In general it showed better accuracy with lower data dispersion. Moreover, the sample preparation is very simple and straightforward, potentially being applicable as a high-throughput method which, on account of its simplicity and low cost, may be applied to the analysis of a large number of samples in the occasion of outbreaks of large-scale contamination.
Mathematic diagnosis of unifloral honeys. A study was carried out to develop suitable statistical... more Mathematic diagnosis of unifloral honeys. A study was carried out to develop suitable statistical methods in order to obtain a mathematic diagnosis of unifloral honeys. Introduzione Per definire le caratteristiche dei mieli uniflorali, sono normalmente impiegati tre approcci analitici, utili per l'identificazione e il controllo dell'origine botanica: l'esame organolettico, microscopico e fisico-chimico. Le analisi sensoriali e microscopiche, per essere correttamente condotte e interpretate, richiedono una competenza ed un'esperienza specifiche da parte dell'analista; quelle fisico-chimiche sono di più semplice esecuzione e di maggiore riproducibilità, ma risentono comunque di una certa difficoltà interpretativa, a causa della grande variabilità del miele che rende difficile fissare precisi limiti di composizione per le diverse tipologie. Attraverso uno studio statistico sono stati individuati i parametri dotati di maggior potere discriminante ed è stata verificat...
International honey standards are specified in a European Honey Directive and in the Codex Alimen... more International honey standards are specified in a European Honey Directive and in the Codex Alimentarius Standard for Honey, both of which are presently under revision. In this paper the present knowledge on the different quality criteria is reviewed. The standard drafts, ...
Although American Foulbrood is well known, this disease is still a relevant cause of beehive and ... more Although American Foulbrood is well known, this disease is still a relevant cause of beehive and economic losses to beekeepers. Gamma radiation from a Cobalt-60 source provides an effective means of treating AFB contaminated beekeeping material for its reuse in apiary. Contaminated equipment (hive, frames, wax, honey) was irradiated at three different dosages: 10, 15 and 25 kGray. The infectivity
ABSTRACT In this study, heavy metal levels detected in molluscs produced in the Veneto Region (no... more ABSTRACT In this study, heavy metal levels detected in molluscs produced in the Veneto Region (north-western Adriatic Sea) are presented and discussed. A descriptive analysis was conducted on data collected in the framework of official monitoring activities in shellfish production areas between 2007 and 2012. Concentrations of lead (Pb), mercury (Hg) and cadmium (Cd) in about 2000 samples of 17 different species of marine bivalve molluscs, echinoderms and gastropods were checked by means of atomic absorption spectrometry. Hg and Pb concentrations were always below the maximum levels set by the European legislation; 2.2% of the analysed samples exceeded the threshold level for Cd, 86.7% of witch belonging to purple dye murex (Bolinus brandaris). The highest mean levels of Hg and Cd were found in purple dye murex, with 0.10 mg kg−1 and 0.88 mg kg−1 respectively, while rayed trough shell (Mactra stultorum) and truncate donax (Donax trunculus) were the species with the highest mean value of Pb (0.25 mg kg−1). Species of major consumption showed mean values almost ten times lower than the limits set by the European legislation (Manila clam: Pb: 0.20 mg kg−1; Hg: 0.04 mg kg−1; Cd: 0.07 mg kg−1; Mediterranean mussel: Pb: 0.22 mg kg−1; Hg: 0.03 mg kg−1; Cd: 0.13 mg kg−1). A preliminary evaluation of the impact on human health of shellfish according to the detected levels indicates that the species of major consumption are safe for the average consumers, although a potential risk cannot be ruled out for vulnerable groups, such as women of childbearing potential and children, as well as for regular or high-level shellfish consumers, particularly those who frequently eat species such as murex.
Honey, in particular monofloral varieties, is a valuable commodity. Here, we present proton trans... more Honey, in particular monofloral varieties, is a valuable commodity. Here, we present proton transfer reaction-time of flight-mass spectrometry, PTR-ToF-MS, coupled to chemometrics as a successful tool in the classification of monofloral honeys, which should serve in fraud protection against mispresentation of the floral origin of honey. We analyzed 7 different honey varieties from citrus, chestnut, sunflower, honeydew, robinia, rhododendron and linden tree, in total 70 different honey samples and a total of 206 measurements. Only subtle differences in the profiles of the volatile organic compounds (VOCs) in the headspace of the different honeys could be found. Nevertheless, it was possible to successfully apply 6 different classification methods with a total correct assignment of 81-99% in the internal validation sets. The most successful methods were stepwise linear discriminant analysis (LDA) and probabilistic neural network (PNN), giving total correct assignments in the external validation sets of 100 and 90%, respectively. Clearly, PTR-ToF-MS/chemometrics is a powerful tool in honey classification.
The applicability of gel permeation chromatography (GPC) to the purification in foodstuffs in the... more The applicability of gel permeation chromatography (GPC) to the purification in foodstuffs in the detection of three classes of drugs, sulfonamides, nitrofurans, and growth promoters, is described. This technique has already found a wide application in the routine analysis of pesticides in milk, eggs and grease but to our knowledge there is no published work on the use of GPC for purifying animal feedstuffs for the detection of the above-mentioned classes of drugs. Three main advantages characterize this method: the simultaneous determination of a wide spectrum of drugs; good performance of the purification system; and high recoveries. The method was tested for a determination limit of 1 ppm in each compound. Average recoveries of spiked samples were: 99% for sulfonamides; 98% for nitrofurans; and 100% for carbadox [methyl-3-(2-quinoxalinylmethylene) carbazate-1,4-dioxide] and olaquindox [N-(2-hydroxyethyl)-3-methyl-2-quinoxalinecarboxamide-1,4-dioxide] . The method was also tested for linearity over the range 1-100 ppm and gave r values between 0.9998 and 0.9999 for each drug. Analyses were performed by HPLC, either using a diode array or windowplot-system detector. The described method is quick and simple, which is very useful in routine analysis.
International Journal of Environmental Analytical Chemistry, 2015
ABSTRACT This work was performed to highlight the advantages of total reflection X-ray fluorescen... more ABSTRACT This work was performed to highlight the advantages of total reflection X-ray fluorescence spectroscopy (TXRF) for multi-elemental qualitative and quantitative analysis of wine. Indeed the International Organization of Vine and Wine (OIV) selected some potentially toxic elements and proposed limit values for their concentration in wines. Direct TXRF analysis of nine wine samples from Emilia Romagna region of Italy was performed in two different laboratories: Italy and Japan. Wine dehydration was also evaluated as sample conservation mean. Traces of Fe, Cu, Zn and Pb are present in all the analysed samples, with concentrations lower than the limits established by the OIV. The target hazard quotients (THQs) were also calculated for seven elements (Cl, Mn, Fe, Ni, Cu, Zn and Sr) to determine their potential detrimental effects. The results show that TXRF is a fast, simple and accurate analytical technique for trace element analysis of wine. Moreover, dehydration is an effective way to store wine samples for further elemental analysis.
A new chromatographic method is proposed for the analysis of aflatoxin M(1) in milk. The method i... more A new chromatographic method is proposed for the analysis of aflatoxin M(1) in milk. The method is based on liquid-liquid extraction followed by LC-MS/MS analysis. Liquid-liquid extraction (LLE) is performed on the defatted milk plus sodium chloride by using ethyl acetate as an extraction solvent. Accuracy and precision were evaluated at the LOQ (15 ng kg(-1)) spiked sample as well as with three other different naturally contaminated reference materials. The mean overall recovery (n = 24) was 95% with a confidence interval of 1.9% and a CV% of 4.5%. The performance of the proposed method was compared with that of the Official ISO Method based on the use of immunoaffinity chromatography columns (IAC): LLE protocol could be considered a valid alternative to the LC-IAC. In general it showed better accuracy with lower data dispersion. Moreover, the sample preparation is very simple and straightforward, potentially being applicable as a high-throughput method which, on account of its simplicity and low cost, may be applied to the analysis of a large number of samples in the occasion of outbreaks of large-scale contamination.
Mathematic diagnosis of unifloral honeys. A study was carried out to develop suitable statistical... more Mathematic diagnosis of unifloral honeys. A study was carried out to develop suitable statistical methods in order to obtain a mathematic diagnosis of unifloral honeys. Introduzione Per definire le caratteristiche dei mieli uniflorali, sono normalmente impiegati tre approcci analitici, utili per l'identificazione e il controllo dell'origine botanica: l'esame organolettico, microscopico e fisico-chimico. Le analisi sensoriali e microscopiche, per essere correttamente condotte e interpretate, richiedono una competenza ed un'esperienza specifiche da parte dell'analista; quelle fisico-chimiche sono di più semplice esecuzione e di maggiore riproducibilità, ma risentono comunque di una certa difficoltà interpretativa, a causa della grande variabilità del miele che rende difficile fissare precisi limiti di composizione per le diverse tipologie. Attraverso uno studio statistico sono stati individuati i parametri dotati di maggior potere discriminante ed è stata verificat...
International honey standards are specified in a European Honey Directive and in the Codex Alimen... more International honey standards are specified in a European Honey Directive and in the Codex Alimentarius Standard for Honey, both of which are presently under revision. In this paper the present knowledge on the different quality criteria is reviewed. The standard drafts, ...
Although American Foulbrood is well known, this disease is still a relevant cause of beehive and ... more Although American Foulbrood is well known, this disease is still a relevant cause of beehive and economic losses to beekeepers. Gamma radiation from a Cobalt-60 source provides an effective means of treating AFB contaminated beekeeping material for its reuse in apiary. Contaminated equipment (hive, frames, wax, honey) was irradiated at three different dosages: 10, 15 and 25 kGray. The infectivity
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Papers by Roberto Piro