Characterization of Final Action Official MethodSM 2011.19 and First Action Official Method 2015.06 Performance at Analyte Levels Corresponding to CODEX STAN 72 (1981) Minimum Levels.

A limited single-laboratory validation (SLV) was conducted in the authors' laboratory to investigate the performance of AOAC Official MethodsSM 2011.19 Determination of Chromium (Cr), Selenium (Se), and Molybdenum (Mo) in Infant Formula and Adult Nutritional Products by Inductively Coupled Plasma/Mass Spectrometry and 2015.06 Determination of Minerals and Trace Elements in Infant Formula and Adult/Pediatric Nutritional Formula by Inductively Coupled Plasma/Mass Spectrometry at analyte levels below the practical LOQs (PLOQs) already published for these Final Action Official Methods. This work was needed to verify that the actual LOQs were below the minimum requirements for minerals in infant formula as given in CODEX STAN 72 (1981). Linearity studies at low levels were conducted as well as the analysis of blanks over multiple days to establish the LOQs (as opposed to PLOQs) for these nutrients. Several placebo matrixes from the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) program were tested over multiple days at two different sample sizes to quantitate the effect of doubling the sample size given in the original publications. The SLV results indicate that both methods can meet the Codex minimum requirements as-is, without modification of the methods, albeit with a relaxation of the stringent precision criteria originally established for these methods by SPIFAN. Precision can be improved by doubling the sample size, but this step is not necessary to use the method for its intended purpose. A concurrent collaborative study of Method 2015.06 showed that the RSDR obtained across eight laboratories for several infant formula placebos containing mineral concentrations between the PLOQ and LOQ were indeed worse than SPIFAN expectations, but reasonable Horwitz ratios (HorRat) were nonetheless obtained for these analytes.

[Atomic absorption fingerprint and identification studies of Da Huo Luo pill. I. Exploration of inorganic elements fingerprint for establishment of industrial standard].

The fingerprints for most of Chinese medicines based on their organic compositions have been well established. Nevertheless, there are very few known fingerprints which are based on inorganic elements. In order to identify the Da Huo Luo Dan and its efficiency from other Chinese medicines, the authors attempted to set up a fingerprint which could be determined by the measurement of inorganic elements in Da Huo Luo Dan and other Chinese medicines. In the present study, the authors first employed 28 batches of Da Huo Luo Dan produced by Zhang-Shu Pharmatheutical Company in Jiang Xi Province to screen 12 kinds of inorganic elements measured by atomic absorption spectrophotometer and established the atomic absorption fingerprints. Secondly, the authors tried to identify Da Huo Luo Dan and other Chinese medicines by using the similarly analysis of vectors and the statistical analysis of compositional data. The result showed that the methods the authors used here were predictable to tell the efficiency of Da Huo Luo Dan from others. The authors' study also proves that establishment of standard for quality control by analysis of inorganic elements in Chinese medicines is feasible. The present study provides a new idea and a new technique that serve for the establishment of industrial standards for analysis of inorganic elements fingerprint to explore the effects of Chinese medicines.

Soil fertility in relation to slope position and agricultural land use: a case study of Umbulo Catchment in southern Ethiopia.

A study was conducted in southern Ethiopia to evaluate the nutrient status on smallholder farms with respect to land use class (garden, grassland, and outfield) and slope position (upper, middle, and lower). Soil physical and chemical properties were quantified using soil samples collected at two depths (0-15 and 15-30 cm). Available phosphorous was significantly different among the three land use classes. However, organic carbon and total nitrogen were lower in the outfield compared to the garden and grass land but not significantly different. The lower than expected nutrient status of the garden and grassland, which receive almost all available organic supplements, was attributed to the overall low availability of these inputs. Similarly, pH and cation exchange capacity were not significantly different among the different land use classes. However, the sum of the exchangeable cations was significantly higher in the garden compared to the outfields. Comparison at landscape level revealed that the sand fraction was significantly greater, whereas the silt fractions were significantly smaller, on the lower slopes relative to the middle slopes. Moreover, the organic carbon, total nitrogen, cation exchange capacity, Ca, and Mg values were significantly less on lower slopes than upper and middle slopes. Perhaps this is because of leaching and the effect of deposition of coarser sediments from the prevailing gully system. Overall, the fertility of the soil was adequate for supporting smallholder farming, but consideration must be given to reducing pressure on the land resources, addressing erosion problems, and providing a line of credit for purchasing inputs.

Effect of evaporation and pasteurization in the biochemical and immunological composition of human milk.

OBJECTIVE: To assess the effects of evaporation and pasteurization of human milk on its biochemical and immunological composition and on its osmolarity. METHODS: The samples of mature human milk were categorized into four study groups: in natura human milk, pasteurized human milk, human milk evaporated at 70% of the baseline volume and human milk pasteurized and evaporated at 70%, with 12 different samples of milk in each group. The samples were used to determine the concentrations of sodium, potassium, calcium, phosphorus, magnesium, protein, fat, lactose, immunoglobulin A and osmolarity. RESULTS: The pasteurization of human milk did not show statistically significant changes in the concentration of sodium, potassium, calcium, phosphorus, magnesium, protein, fat, lactose, or in osmolarity; however, it showed remarkable reduction in the mean concentration of immunoglobulin A. Evaporation had a mean increase of 38% in the concentration of sodium, potassium, calcium, phosphorus, magnesium, protein, fat and lactose and mean reduction of 45% in the concentration of immunoglobulin A, without significant change in osmolarity in unprocessed milk. CONCLUSION: By evaporation at 70% of the baseline value of human milk, it is possible to obtain human milk that meets the nutritional requirements recommended for preterm infants, except for calcium and phosphorus.

Effect of evaporation and pasteurization in the biochemical and immunological composition of human milk

OBJETIVO: Avaliar os efeitos da evaporação e da pasteurização do leite humano na sua composição bioquímica e imunológica e em sua osmolaridade. MÉTODOS: As amostras de leite humano maduro foram divididas em quatro grupos de estudo: leite humano in natura, leite humano pasteurizado, leite humano evaporado a 70 por cento do volume inicial e leite humano pasteurizado e evaporado a 70 por cento, com 12 diferentes amostras de leite em cada grupo. Das amostras dos grupos, foram dosadas as concentrações de sódio, potássio, cálcio, fósforo, magnésio, proteína, gordura, lactose, imunoglobulina A e osmolaridade. RESULTADOS: A pasteurização do leite humano não mostrou alterações estatisticamente significantes na concentração dos elementos sódio, potássio, cálcio, fósforo, magnésio, proteína, gordura, lactose, nem na osmolaridade; no entanto, mostrou redução significante na concentração média de imunoglobulina A. A evaporação mostrou aumento estatisticamente significativo de 38 por cento em média na concentração dos elementos sódio, potássio, cálcio, fósforo, magnésio, proteína, gordura e lactose e redução média de 45 por cento na concentração da imunoglobulina A, sem alteração significativa da osmolaridade em relação ao leite sem processamento. CONCLUSÃO: Através da evaporação a 70 por cento do volume inicial do leite humano, pode ser obtido leite humano com condições de satisfazer as necessidades nutricionais preconizadas para o recém-nascido pré-termo, com exceção do cálcio e do fósforo.

OBJECTIVE: To assess the effects of evaporation and pasteurization of human milk on its biochemical and immunological composition and on its osmolarity. METHODS: The samples of mature human milk were categorized into four study groups: in natura human milk, pasteurized human milk, human milk evaporated at 70 percent of the baseline volume and human milk pasteurized and evaporated at 70 percent, with 12 different samples of milk in each group. The samples were used to determine the concentrations of sodium, potassium, calcium, phosphorus, magnesium, protein, fat, lactose, immunoglobulin A and osmolarity. RESULTS: The pasteurization of human milk did not show statistically significant changes in the concentration of sodium, potassium, calcium, phosphorus, magnesium, protein, fat, lactose, or in osmolarity; however, it showed remarkable reduction in the mean concentration of immunoglobulin A. Evaporation had a mean increase of 38 percent in the concentration of sodium, potassium, calcium, phosphorus, magnesium, protein, fat and lactose and mean reduction of 45 percent in the concentration of immunoglobulin A, without significant change in osmolarity in unprocessed milk. CONCLUSION: By evaporation at 70 percent of the baseline value of human milk, it is possible to obtain human milk that meets the nutritional requirements recommended for preterm infants, except for calcium and phosphorus.

Distribution of elements in needles of Pinus massoniana (Lamb.) was uneven and affected by needle age.

Macronutrients (P, S, K, Na, Mg, Ca), heavy metals (Fe, Zn, Mn, Cu, Pb, Cr, Ni, Cd) and Al concentrations as well as values of Ca/Al in the tip, middle, base sections and sheaths of current year and previous year needles of Pinus massoniana from Xiqiao Mountain were analyzed and the distribution patterns of those elements were compared. The results indicated that many elements were unevenly distributed among the different components of needles. Possible deficiency of P, K, Ca, Mn and Al toxicity occurred in needles under air pollution. Heavy metals may threaten the health of Masson pine. Needle sheaths were good places to look for particulate pollutants, in this case including Fe, Cu, Zn, Pb, Cr, Cd and Al.

The importance of atmospheric deposition, charge and atomic mass to the dynamics of minor and rare elements in developing, ageing, and wilted leaves of beech (Fagus sylvatica L.).

The amounts of sixty elements in developing, maturing, senescent and wilting leaves, and in the wintering dead leaves attached to the branches, are reported for a beech (Fagus sylvatica) forest on mor Podzol in south Sweden, a site with no local sources of pollution or geological anomalies. The amounts (contents per leaf) of K (potassium), Rb (rubidium), Cs (caesium), Cu (copper) and P (phosphorus) were highest in young leaves, decreasing throughout the growing season and usually in the subsequent winter. The entirely opposite pattern with a continuous, mostly even increase of the amounts was measured with Be (beryllium), Ba (barium), Hg (mercury), Al (aluminium), Tl (thallium), Pb (lead), Bi (bismuth), V (vanadium), W (tungsten), As (arsenic), Sb (antimony), and Se (selenium). Amounts of rare-earth elements and some transition metals, such as Co (cobalt), Ti (titanium), and the actinides Th (thorium) and U (uranium) were more stable during the growing season, after an initial increase in early summer, but increased greatly in the winter. This winter increase in dead attached leaves has to be accounted for by uptake from long-distance transported constituents in dry and wet deposition. It was similar to deposition rate estimates using moss carpets from the same locality. A passive uptake was positively related to ionic charge and atomic mass. However, the amounts of several, mainly non-essential elements, such as Ni (nickel), Sc (scandium), Zr (zirconium), Cr (chromium), Ag (silver), and Cd (cadmium) were not much lower in the young or maturing leaves than in the wintered dead leaves of this deciduous (hardwood) forest and a proportion apparently originated from internal translocation in the trees. Seasonal fluxes or cycling of many of the scarce or rare elements reported here have never been studied before in forest ecosystems.

Concentration levels of major and trace elements in rice from Sri Lanka as determined by the k0 standardization method.

Instrumental neutron activation (INAA) with k0 standardization has been used to determine the concentration levels of a variety of major and trace elements (Al, As, Br, Cd, Cl, Co, Cr, Cs, Cu, Fe, Hg, K, La, Mg, Mn, Mo, Na, Rb, Sc, Se, and Zn) in rice grains (raw and parboiled) and in rice flour collected from local markets in Sri Lanka. In addition, the energy-dispersive X-ray fluorescence (EDXRF) analysis has been used to determine the three elements Ca, P, and S in powdered samples. To evaluate and assure the accuracy and precision of the k0 standardization method, the IAEA standard reference material V-8 rye flour was analyzed. The results obtained in the present investigation were compared with the results reported from other countries. All of the elements detected in the rice matrices from Sri Lanka were very low in concentration or within normal limits for food plants. Approximate daily dietary intakes of the individual elements supplied through rice were calculated and compared with the available literature values of daily allowances.

Concentrations of major elements and mercury in unstimulated human saliva.

The aim of this study was a preliminary assessment of a possible role of human saliva in the diagnosis of some physiological and pathological changes in oral and body functions. Reliable procedures for collection and analysis of samples were established in order to assess total concentrations of Ca, K, Mg, Na, P, and Hg in whole unstimulated saliva. Possible relationships between element concentrations and sex, age, smoking, illness conditions, or side effects resulting from the use of drugs were investigated. The effects of stimulated or unstimulated collection procedures, dental prosthesis, and amalgam fillings were also evaluated. Total concentrations of major cations and Hg in whole saliva from 33 healthy adults living in the Siena district showed a coefficient of variation ranging from 11% (P) to 53% (Na) and average values were in the same range of those previously reported for unstimulated saliva. Healthy males had significantly higher concentrations of K, Na, P, and Na/K, Na/Ca, Na/Mg, and Na/P values than females. Age, smoking, dental prosthesis, and amalgam fillings had no significant effects on the concentrations of major elements. On the contrary, concentrations of Hg were positively correlated to the number of amalgam fillings and increased at a rate of about 1.9 microg/L for each filling. No correlations were found between Hg concentrations and those of major elements. Comparisons with literature data showed a different composition (particularly for Na and Hg concentrations) between unstimulated and stimulated saliva. Samples from patients affected by idiopathic pulmonary fibrosis had significantly higher concentrations of K and the maximum value was measured in a patient affected by acute pulmonary edema. This increase was likely the result of pharmacological treatments with tricyclic antidepressants and/or saline solutions. Data reported in this study, although preliminary, contribute to the assessment of levels of major cations (some of them very little investigated) and Hg in whole unstimulated human saliva and provides consistent support for further research on the possible use of this easy accessible matrix as a diagnostic tool of body function changes.

Simultaneous determination of inorganic and organic anions, alkali, alkaline earth and transition metal cations by capillary electrophoresis with contactless conductometric detection.

Simultaneous separation of up to 22 inorganic and organic anions, alkali, alkaline earth and transition metal cations was achieved in less than 3 min in the capillary electrophoresis system with contactless conductometric detector. The sample was injected from both capillary ends (dual opposite end injection) and anionic and cationic species were detected in the center of the separation capillary. The parameters of the separation electrolyte, such as pH, concentration of the electrolyte, concentration of complexing agents and concentration of 18-crown-6 were studied. Best results were achieved with electrolytes consisting of 8 mM L-histidine, 2.8 mM 2-hydroxyisobutyric acid, 0.32 mM 18-crown-6 at pH 4.25 or 9 mM L-histidine, 4.6 mM lactic acid, 0.38 mM 18-crown-6 at pH 4.25. Other electrolytes containing complexing agents such as malic or tartaric acid at various concentrations could also be used. The detection limits achieved for most cations and anions were 7.5 - 62 micro gL(-1) except for Ba2+ (90 micro gL(-1)), Cd 2+, Cr 3+ and F- (125 micro gL(-1)), and fumarate (250 micro gL(-1)). The repeatability of migration times and peak areas was better than 0.4% and 5.9%, respectively. The developed method was applied for analysis of real samples, such as tap, rain, drainage and surface water samples, plant exudates, plant extracts and ore leachates.

[Simultaneous analysis of alkali metals and alkaline earth metals in Chinese herbal medicine by ion chromatography].

A simple and rapid method for the analysis of cations by using ion chromatography was developed. The results showed that the content ratio of Na+, NH4+, K+, Mg2+, Ca2+ in rhizoma chuanxiong and semen zizyphi spinosae are different. The detection limits of cations (S/N = 3) were 0.001-0.013 mg/L. The calibration curves of peak areas for all analytes were linear over two or three orders of magnitude with a regression coefficient (r2) of 0.9995-1.0000.