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RATIONALE: The oxygen and hydrogen isotope compositions of the water component of the milk from nine Italian dairy farms were studied together with the farm water for one year. The aim was to verify the importance of farm water and seasonal temperature variation on milk isotope values and propose mathematical relations as new tools to identify the milk origin. METHODS: Milk was centrifuged to separate the solids and then distilled under vacuum to separate water. δ(18 O/16 O) and δ(2 H/1 H) analyses of the water molecules were carried out using a water equilibrator online with a mass spectrometer. For oxygen and hydrogen isotope determination, water was equilibrated with pure CO2 for 7.5 h and with pure H2 for 5 h, respectively. The isotope ratio value is indicated with δ (expressed on the VSMOW/SLAP scale) as defined by IUPAC. RESULTS: The average annual isotope value of milk at the different cattle sheds is mostly related to the farm water suggesting that the drinking water is the most important factor influencing the isotopic values of the milk water. The milk/water fractionation factor correlates with the milking time and, thus, the seasonal temperature is best described by a 4th order polynomial regression line. A two-level check model was used to verify the milking provenance. CONCLUSIONS: This study shows that it is essential to analyze both milk and farm water to indicate provenance. A two-step verification tool, based on the difference between the measured and calculated δ(18 O/16 O)M values, and the difference between the calculated and estimated milk-water fractionation factors, allowed the source determination of milk. Both conditions must be met if the milk is considered to be from the Parmigiano-Reggiano production region. Although this approach was developed for this region, it can easily be tested and adapted to other dairy production areas.
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Deutério/análise , Água Doce/química , Leite/química , Isótopos de Oxigênio/análise , Animais , Bovinos , Análise Discriminante , Fazendas , Feminino , Itália , Espectrometria de Massas , Controle de Qualidade , Estações do AnoRESUMO
RATIONALE: Oxygen isotope analysis of water molecules of liquid foodstuffs is commonly performed under isotopic equilibrium between water in the solution and the vapour water, assuming that the liquid water activity is equal to unity and that liquid water is an ideal mixture of H2 O isotopologues. A priori this behaviour is not realistic for all foodstuffs, which frequently are very concentrated solutions. In this paper we mainly consider "balsamic vinegar" with the aim of defining an appropriate procedure of oxygen isotope ratio analysis of water molecules in these concentrated solutions. METHODS: Isotope ratio mass spectrometry (IRMS) measurements of the oxygen isotope ratios (δ18 O values) were carried out on CO2 equilibrated with water molecules at 22 ± 0.1°C. Three independently calibrated, very low salinity waters were used as standards. RESULTS: For grape must and wine vinegar (density < 1.15 g/cm3 ) the δ18 O values for water determined directly on these solutions are "true" values. On the contrary, for balsamic vinegar with density higher than 1.15-1.20 g/cm3 , the δ18 O values obtained directly on the solutions are systematically different from those obtained on water produced by distillation of the same samples at 70°C under vacuum. CONCLUSIONS: In the case of balsamic vinegar with density higher than 1.15-1.20 g/cm3 , to avoid severe systematic errors, the isotopic analyses must be carried out on water obtained by distillation under stirring.
Assuntos
Análise de Alimentos/métodos , Isótopos de Oxigênio/análise , Água/química , Ácido Acético/química , Análise de Alimentos/normas , Espectrometria de Massas/métodos , Modelos Químicos , Isótopos de Oxigênio/química , Reprodutibilidade dos Testes , Gravidade Específica , Vitis/químicaRESUMO
OBJECTIVES: A contribution to the knowledge of the economy and the environmental surroundings of the populations living along the Nile valley in three different periods. MATERIALS AND METHODS: This study reports stable isotope analyses on apatite bone samples of 139 humans, 48 mammals, and 43 fish from the Al Khiday archaeological sites in Sudan. The bones belong to four archaeological periods: pre-Mesolithic, Mesolithic, Neolithic, and Meroitic. Data were processed statistically. RESULTS: A significant difference exists between the pre-Mesolithic and Mesolithic mean δ(18) Ow value and the mean of the modern Nile. The mean δ(18) Ow values for the Neolithic humans and bovids are very similar (+1.5 ±4, and -2, respectively) and more positive than the mean values of Mesolithic mammals and Pre-Mesolithic humans. The water ingested by Meroitic humans (+7 ± 2.5) is enriched in (18) O in respect to the water ingested by the Neolithic population. There is a separation in the δ(13) Cdiet values between the pre-Mesolithic humans (-14 ± 1) and Mesolithic mammals (-12 ± 2) group and the Neolithic humans (-18 ± 1), Meroitic humans (-19 ±1), Neolithic mammals (-21), and the modern (mean δ(13) Cdiet = -19 ±2) mammal group. DISCUSSION: The climate became warmer and more arid from the pre-Mesolithic/Mesolithic to the Meroitic period. The environmental conditions influenced the strategies of subsistence and, in particular, the changes occurring from the pre-Mesolithic to the Neolithic can be considered contemporaneous to the transition from hunting-gathering-fishing to cultivation-herding. Am J Phys Anthropol 160:498-518, 2016. © 2016 Wiley Periodicals, Inc.