Papers by Maurizio Bettinelli
A Ancora una volta a rontiamo il complesso tema della taratura, processo così essenziale ai ni di... more A Ancora una volta a rontiamo il complesso tema della taratura, processo così essenziale ai ni di una buona analisi di laboratorio, eppure ancora così poco compreso nella sua natura più profonda. Tra i tanti i motivi che concorrono a rendere così complessa la questione vi sono: quello normativo, lessicale e formativo. Ci proponiamo, quindi, di approfondire proprio questi aspetti, cercando di chiarirli il più possibile… sperando di contribuire a dipanare la matassa. Gli aspetti più spinosi Come già rilevato da una precedente inchiesta, la norma UNI EN ISO 10012:2004 «non è ancora stata compresa nella sua natura più profonda da molti laboratori di analisi italiani» specificano Maurizio Bettinelli, chimico libero professionista, presidente della Società italiana valori di riferimento (SIVR) e ispettore tecnico Accredia e l'ingegner Mario Mosca, Direttore del Dipartimento Laboratori di Taratura di Accredia-DT. «La UNI EN ISO 10012:2004 è una guida che, nell'ottica delle precedenti UNI EN ISO 9001 e UNI EN ISO 14001, dice come utilizzare al meglio la strumentazione presente in Azienda e quindi anche in laboratorio» afferma l'ingegner Mosca. «Si tratta di una norma di sistema, il cui scopo è, in ultima analisi, ridurre il rischio Aziendale di fornire al cliente risultati che
There are more things in heaven and earth, Horatio, than are dreamt of in our philosophy.
Uranium analysis in fish, echinoderms and shellfish samples collected in the north part of the Ad... more Uranium analysis in fish, echinoderms and shellfish samples collected in the north part of the Adriatic Sea is presented. The aim of the work was to evaluate uranium concentrations in samples of this kind, and also to investigate possible contamination from depleted uranium (DU) in consequence of the war operations previously conducted in that area. DU contamination was checked by measuring the 235 U/ 238 U isotope ratio. The samples were dissolved according to the EPA 3052 procedure , and the determinations were performed by inductively coupled plasma mass spectrometry (ICP-MS), optimized in order to perform isotope ratio measurements with good precision. The method was validated by evaluating the recovery from spiked samples; results in the range 93– 107% were obtained. The isotope ratio measurement was evaluated in terms of accuracy and precision by analyzing the certified reference materials IAEA 326 and GBW 07305, and good agreement with the certified values was obtained here also. The concentration of uranium was higher in invertebrate samples than in fish (0.3–2 mg/g of U vs. 0.05–0.1 mg/g, respectively). The isotope ratio measurements for all the samples gave values very similar to the natural ratio, permitting exclusion of the presence of DU.
Atomic Spectroscopy Norwalk Connecticut, 1983
Trace Elements and Electrolytes, 2013
Trace Elements and Electrolytes, 2013
Clinica Chimica Acta, 1985
dcabc.uniba.it
... PL 8. Treatment of the rest fraction of household waste in Flanders novel developments. Van... more ... PL 8. Treatment of the rest fraction of household waste in Flanders novel developments. Vandecasteele Carlo 1 , Van Gerven Tom 1 , Wauters Guido 2. 1 Chemical Engineering Department, KULeuven, de Croylaan 46, 3001 Leuven, Belgium; ...
Microchemical Journal, Oct 1, 2002
Lichens are currently used as bioindicators to monitor air pollution and to follow changes in pol... more Lichens are currently used as bioindicators to monitor air pollution and to follow changes in pollution patterns. In order to perform reliable biomonitoring, the analysis should be accurate, which implies that a good quality control system should be applied. One way to achieve accuracy is to use analytical procedures validated with certified reference materials (CRM) and tested on real samples by comparing different instrumental techniques. In this paper, a microwave digestion procedure developed for determining several elements in lichen samples by ICP-OES, GFAAS and ICP-MS is described. Among other usual mixtures of attack (HNO and H O ) it also includes the use of HF in 3 2 2 order to assure the complete solubilization of atmospheric particulate or soil dust present on the surface of biomonitors. The method was tested on CRM 482 Pseudovernia furfurea, with good recoveries for approximately 20 elements, and by analyzing real samples in different laboratories with different analytical techniques. The aim of the present work was to demonstrate that the enrichment factor (EF) used in biomonitor programs can be estimated in a correct way only adopting a complete solubilization of the lichen samples, which assures accurate results independently from the presence of atmospheric particulate of different origin and morphology. ᮊ
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Giornale italiano di medicina del lavoro ed ergonomia
According to recently issued (UNI CEI EN ISO/IEC 17025, UNI CEI ENV 13005 and prEN ISO 15189) sta... more According to recently issued (UNI CEI EN ISO/IEC 17025, UNI CEI ENV 13005 and prEN ISO 15189) standards, to assure the quality of analytical results and their comparability in time and in different places, testing and clinical laboratories must demonstrate to use validated methods, guarantee the traceability of their measurements and state the measurement uncertainty associated with each result. For some SI quantities, such as the mass, the traceability to SI and the estimate of measurement uncertainty are warranted by established methods. In the clinical laboratory and especially in preventive, environmental and occupational laboratory medicine, specific difficulties arise to warrant the traceability to the mole. On one hand, the whole concept of measurement uncertainty is new in laboratory medicine, on the other hand, its application faces practical difficulties, because of the wideness and the complexity of the analytical repertory, the lack of officially validated methods and matrix-specific reference materials traceable to SI. In this paper we discuss briefly the concept of measurement uncertainty and its meaning in comparison with other parameters used to define the performance of analytical methods. In addition, we describe the procedures recommended by international organisations for estimating measurement uncertainty and interpreting analytical results with an associated measurement uncertainty in comparison with limit values.
Parole chiave: incertezza di misura, riferibilità, medicina di laboratorio.
Atomic Spectroscopy -Norwalk Connecticut-
The rare earth element (REE) concentration in tomato plants and soils of three agricultural farms... more The rare earth element (REE) concentration in tomato plants and soils of three agricultural farms in the Province of Piacenza, Italy, was evaluated. The REE distribution in the different parts of the plant follows the order: root > leaf > stem > edible part; the concentrations reflect those observed in the soil. The most reliable REE concentrations are obtained from soil having the lowest pH and organic matter. The analytical procedure, using inductively coupled plasma mass spectrometry (ICP-MS), proved to be suitable for the determination of REEs in plants and soil, and was validated using certified samples. The precision of the method resulted in better than 10-15% for all REEs, with recoveries ranging from 70-150%. The method detection limit was 10 ng/g for soil and 1 ng/g for plant material. This technique seems to be promising for its application in tracing REE concentrations in tomato plants and its use in ensuring high quality of typical food products.
The Determination of Chemical Elements in Food, 2007
... 77, 29100 Piacenza, Italy, E-mail: maurizio.bettinelli@libero.it S. SPEZIA, A. GATTI, A. RONC... more ... 77, 29100 Piacenza, Italy, E-mail: maurizio.bettinelli@libero.it S. SPEZIA, A. GATTI, A. RONCHI, AND C. MINOIA Laboratory for Environmental and Toxicological Measurements, S. Maugeri Foundation, Via Ferrata 8, 27100 Pavia, Italy C. ROGGI AND G. TURCONI Department of ...
Rapid Communications in Mass Spectrometry, 2004
A sensitive, accurate and reproducible procedure has been developed for the quantitative determin... more A sensitive, accurate and reproducible procedure has been developed for the quantitative determination of gemcitabine (2 0 ,2 0 -difluorodeoxycytidine, dFdC) and its metabolite 2 0 ,2 0 -difluorodeoxyuridine (2dFdU) in human urine. The samples (2 mL) were extracted by solid-phase extraction (SPE) and analyzed by reversed-phase high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC/MS/MS), operating in multiple reaction monitoring (MRM mode). This procedure was validated using 2 0 -deoxycytidine as internal standard (IS). The urine assay was linear over the range 0-50 mg/L, with a limit of quantification (LLOQ) of 0.2 mg/L for gemcitabine and 1.0 mg/L for the metabolite. The respective limits of detection (LODs) for dFdC and 2dFdU were 0.05 and 0.3 mg/L. The precision and accuracy of the assay were determined on three different days. The within-series precision was found to be always less than 8.5 and 12.7% for gemcitabine and 2dFdU, respectively. The overall precision expressed as relative standard deviation (CVr) was always less than 7.1% for both analytes. The recovery of gemcitabine was always greater than 90% with a CVr <6.3%. The measurement uncertainty determined from the validation data assessed the possibility of determining this drug and its metabolite at trace levels in urine, considering that the combined uncertainty of the whole procedure was always less than 30%.
Rapid Communications in Mass Spectrometry, 2003
A direct, rapid and selective method for the quantitative determination of the ethylenethiourea (... more A direct, rapid and selective method for the quantitative determination of the ethylenethiourea (ETU) in human urine has been validated and is reported in the present study. It allows the accurate quantification of ETU in this complex matrix without the use of any internal standard as the sample cleanup is effective enough for the removal of interferences that could lead to ion suppression in the electrospray ionization (ESI) source. This simple and rapid purification system, based on the use of a Fluorosil phase of a BondElut column followed by a liquid-liquid extraction procedure, achieves mean extracted recoveries, assessed at three different concentrations (2.5, 10.0, and 25.0 microg/L), always more than 85%. High-performance liquid chromatography (HPLC) with positive ion tandem mass spectrometry, operating in selected multiple reaction monitoring (MRM) mode, is used to quantify ETU in human urine. The assay is linear over the range 0-50 microg/L, with a lower limit of quantification (LOQ) of 1.5 microg/L and a coefficient of variation (CV) of 8.9%. The lower limit of detection (LOD) is assessed at 0.5 microg/L. The overall precision and accuracy were determined on three different days. The values for within- and between-day precision are &amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;lt; or = 8.3 and 10.1%, respectively, and the accuracy is in the range 97-118%. The relative uncertainties for the LOQ and QC concentrations have been estimated to be 18 and 8%, respectively. The assay was applied to quantify ETU in human urine from growers that regularly handle ethylenebisdithiocarbamate pesticides in large crop plantations. The biological samples were collected at the start and end of the working day, and the ETU urine levels were found to vary between 1.9 and 8.2 microg/L.
Rapid Communications in Mass Spectrometry, 2004
Health-care workers handling antineoplastic agents may be exposed to extremely low doses of these... more Health-care workers handling antineoplastic agents may be exposed to extremely low doses of these drugs. Very sensitive and specific analytical methods are therefore needed for biological monitoring. The aim of this study was to develop and validate a method for trace level determination of doxorubicin, epirubicin, daunorubicin and idarubicin in human urine, using epi-daunorubicin as an internal standard. Solid-phase extraction (SPE) was used for sample preparation. Urine samples were loaded onto Bond Elut C18 cartridges. The analytes were eluted in methylene chloride/2propanol (1:1, v/v) and then evaporated to dryness. The residue was reconstituted with the mobile phase prior to high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/ MS) analysis. Quantitation of each analyte was performed using the multiple reaction monitoring (MRM) method. The urine assay was linear over the range 0.1-2.0 mg/L, with a lower limit of quantification (LLOQ) of 0.10 mg/L for doxorubicin and epirubicin, and 0.03 mg/L for daunorubicin and idarubicin. The respective limits of detection (LODs) were 0.04 and 0.01 mg/L. The precision and accuracy of the assay were determined on three different days. The within-series precision was found to be always less than 13.9% for all the analytes. The overall precision expressed as relative standard deviation (RSD) was always less than 10.6%. The recovery of anthracyclines was assessed at two concentrations of the range tested (0.1 and 2.0 mg/L) and it ranged from 87.7% (daunorubicin) to 102.0% (doxorubicin) and from 79.1% (daunorubicin) to 90.7% (idarubicin) for the lower and the higher level, respectively, with a RSD always less than 9.1%. The uncertainty of the present assay was also evaluated and the combined uncertainty was always less than 20% over all the days of the validation study. This is the first method that makes use of LC/MS/MS for the biological monitoring of occupational exposure to anthracyclines.
Rapid Communications in Mass Spectrometry, 2004
A rapid screening method, previously developed and validated for the determination of 60 PCB cong... more A rapid screening method, previously developed and validated for the determination of 60 PCB congeners in human serum by using high-resolution gas chromatography coupled with low-resolution mass spectrometry, was applied to the establishment of the reference values in the general population. The reliability of this method was further confirmed by analyzing ten serum samples, obtained from the same population group involved in the original study, by electron impact ionization with either low-or high-resolution mass spectrometry. Analyses in electron capture negative ionization mode were also performed for the determination of 'dioxin-like' isomers. The data were found to be in good accordance with one another, especially for the congeners of highest environmental significance. Then, 162 real serum samples were analyzed for the presence of PCBs. Comparison with the results from other studies reported in the literature showed that a similar profile was observed; the most abundant congeners were #153, #180, #138 and #170. A statistical analysis was performed to determine whether there were significant correlations between PCB concentrations and specific variables such as age, gender, and dietary habits.
Rapid Communications in Mass Spectrometry, 2004
Uranium analysis in fish, echinoderms and shellfish samples collected in the north part of the Ad... more Uranium analysis in fish, echinoderms and shellfish samples collected in the north part of the Adriatic Sea is presented. The aim of the work was to evaluate uranium concentrations in samples of this kind, and also to investigate possible contamination from depleted uranium (DU) in consequence of the war operations previously conducted in that area. DU contamination was checked by measuring the 235 U/ 238 U isotope ratio. The samples were dissolved according to the EPA 3052 procedure, and the determinations were performed by inductively coupled plasma mass spectrometry (ICP-MS), optimized in order to perform isotope ratio measurements with good precision. The method was validated by evaluating the recovery from spiked samples; results in the range 93-107% were obtained. The isotope ratio measurement was evaluated in terms of accuracy and precision by analyzing the certified reference materials IAEA 326 and GBW 07305, and good agreement with the certified values was obtained here also. The concentration of uranium was higher in invertebrate samples than in fish (0.3-2 mg/g of U vs. 0.05-0.1 mg/g, respectively). The isotope ratio measurements for all the samples gave values very similar to the natural ratio, permitting exclusion of the presence of DU.
Rapid Communications in Mass Spectrometry, 2002
A method was developed for the determination of rare earth elements (REEs) in urine with electrot... more A method was developed for the determination of rare earth elements (REEs) in urine with electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICPMS). The undiluted sample was directly injected into the graphite tube and trifluoromethane (Freon-23) was used as chemical modifier in order to reduce the vaporization temperature and the memory effect of most of the lanthanides. The detection limits were in the range 1-10 ng/L with relative standard deviation of 3-5% at concentration levels of 1microg/L, and less than 10-15% at 100 ng/L. Two different procedures, external calibration and a standard additions method, were evaluated to measure the concentration levels of lanthanides in the urine samples and the second procedure was considered to be the best choice for calibration in this work. The level of REEs in urine of 50 healthy volunteers was in the range 5-20 ng/L, above the detection limit of ETV-ICPMS.
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Papers by Maurizio Bettinelli