奶粉中5种营养元素的微波消解火焰原子吸收测定法

目的建立奶粉中5种营养元素的火焰原子吸收测定方法。方法利用微波消解处理样品，火焰原子吸收法测定奶粉中钙、镁、铁、锌、铜。结果方法检出限在0．050～0．11μgml，平均回收率为92．8％-103％，样品进行6次平行测定，RSD为0．56％～2．31％。结论方法具有快速、简便、灵敏、准确的优点，适于奶粉中5种营养元素的测定。

灰树花中铁的存在形态分析

优化灰树花中铁元素的提取工艺,对灰树花水提液中微量元素铁进行含量测定及形态分析,分别用0.45μm滤膜、D101大孔吸附树脂,将灰树花水提液中铁分为悬浮态和可溶态、有机态和无机态,并对有机态中蛋白结合态、多糖结合态进行分离。结果表明:灰树花中铁元素最佳提取工艺为温度100℃、时间120min、料液比1:60(g/mL),在此条件下,灰树花中铁提取率(水提液)约72.7%,其中可溶态大约占总量的64.4%,悬浮态大约占总量的8.3%;可溶态中无机态约占总量的39.0%,有机态约占总量的26.1%;有机态则多以蛋白结合态和多糖结合态形式存在,分别占到了总量的12.8%和10.5%。

Primary Speciation Analysis on 6 Kinds of Microelements in Glycyrrhiza uralensis Fisch.

[Objective]The aim was to analyze the primary speciation of 6 microelements in Glycyrrhiza uralensis Fisch. and provide theoretical basis for explaining pharmacodynamic principle of liquorice and discussing quality control of liquorice planting. [Method]The 6 elements Cu,Zn,Ca,Fe,Mg and Mn in roots of G.uralensis were extracted based on traditional decoction method and were separated into water-soluble state and suspension state by micro porous filtering film. The elements in water-soluble state were detected by flame atomic adsorption spectrophotometry （FAAS）. [Result]The results showed that extractive rates of the elements were in the range of 1.71%-60.06%,and immerse-residue ratio in 0.018 3-1.682 0; the results also indicated that the immerse-residue ratio of Zn was biggest （1.68）,Zn played an important medical role and might be considered as the best characteristic element in G.uralensis; the recoveries of the elements were ranged from 95.72% to 103.15% and relative standard deviations （RSD） were less than 2.38%. [Conclusion]Because of its high accuracy,FAAS method is feasible for analyzing primary speciation of microelements in G.uralensis.

Determination of Ca,K,Mg and Fe in Four Fish Species by FAAS

A method for determining calcium （Ca）, potassium （K）, magnesium （Mg） and iron （Fe） in four fish species was opti- mized and validated. It included microwave mineralization of the samples and subsequent quantification by flame atomic absorption spectroscopy （FAAS） with Zeeman-effect background correction. Using HNO3 （65%） and H202 （33%） as extraction solutions, the optimal conditions of extraction were established as follows： 0.5 g of sample mass; microwave time program of 300 W/5 min and 600 W/5 min. The method was free of matrix interferences. The linear correlation coefficients were ≥0.9991, the recovery percentage of analytes was from 99.31% to 103.70% and the RSD （relative standard deviation） was lower than 2.06%. The detection limits obtained were 32.3, 43.2, 14.0 and 68.6ng mL^-1 for Ca, K, Mg and Fe in FAAS respectively. It is shown that the method is rapid, simple, sensitive and accurate. The method was applied to the studies of digestibility and measurement of these nutrients in samples of fish collected from Norway, Japan and China.

Comparison between sequential and single extraction procedures for metal speciation in fresh and dried Sedum Plumbizincicola

Sequential and single extraction procedures were applied to both fresh and dried Sedum Plumbizincicola leaves and stems.The extractants, different from those of soil, sediment or sewage sludge metal fractions, were water, 80%(v/v) ethanol, 1 mol/L Na Cl,2% HAc and 0.6 mol/L HCl. Zn, Cd and Cu in the extracts and samples were measured by flame atomic adsorption spectrometry. In sequential extraction procedures, water soluble form and ethanol soluble form are the main fractions for Zn, while water soluble form and Na Cl soluble form for Cd, and comparatively uniform distribution for Cu with the residue form most and HCl soluble form second. Single extraction procedures are used to compare the extraction efficiencies of the five reagents to screen appropriate extractants and operating conditions for liquid extraction to deal with large amount of harvested metal-contained biomass, which will pose a threat to the environment if treated improperly. The sequences of extraction efficiencies are HCl>Na Cl≈HAc>Water≈Ethanol for Zn and HCl≈Na Cl≈HAc>Water>Ethanol for Cd. As for Cu, all the five extractants cannot effectively extract Cu, but HCl achieves a higher efficiency(>70% in fresh samples, and 45%-60% in dried samples). Besides, extraction efficiencies for most extractants in fresh samples are higher than those in dried samples, and extraction efficiencies of stems and leaves for the five extractants are close. The two extraction procedures can obtain high degree of accuracy with the relative standard deviation(RSD)lower than 10%, and metal recoveries are controlled between 80%-120% with most of 90%-110%.

The Use of Multiwalled Carbon Nanotubes Mini Column for Preconcentration of Trace Metal Ions in Tap Water of Khartoum City and Their Determination by Flame Atomic Absorption Spectrometry （FAAS）

The adsorption behavior of multiwalled carbon nanotubes （MWNTs） toward heavy elements has been investigated systemically, and a new method has been developed for the determination of trace elements in water samples based on preconcentration with mini-column packed with MWNTs prior to its determination by flame atomic absorption spectrometry （FAAS） The recommended parameters of proposed method influencing the preconcentration of the analytes, such as pH of the sample, sample flow rate and volume, elute solution and interfering ions, have been used. Under the optimized conditions, the calibration graphs were linear with the correlation coefficient range 0.9981-0.9995. According to the results, the metals were found 0.019-0.051, 0.011-0.031, 0.00-0.081, 0.00-0.0002, 0.007-0.0925, 0.00-0.0104 μg/L in water samples for Pb, Mn, Zn, Cd, Fe, Cu respectively. The percentage relative standard deviation （%RSD） for five replicate samples were 〈 5% in all cases. The method has been successfully applied to the determination of trace elements in some environmental samples with satisfactory results.

Detection of Total Phenols, Essential and Toxic Elements in Latvian Whole Grain Bread

A survey was carried out with the aim of assessing the level of the total phenolic compounds （TPC）, essential （Na, K, Ca, Mg, Cu, Zn） and toxic （Cd and Pb） elements in 10 Latvian whole grain rye and/or wheat flour bread samples, obtained from the local market. The quantities of the TPC were determined by spectrophotometry. Mineral content was determined by flame photometry, flame atom absorption spectrometry （FAAS） and electrothermal atomic absorption spectrometry （ETAA） after wet digestion in concentrated HNO3. The values were comparable to the literature data. The average content in all the samples was （on a basis of weight of the product） 547 ± 28 mg/100 g for Na; 280 ±20 mg/100 g for K; 32 ± 2 mg/100 g for Ca; 88 ±5 mg/100 g for Mg; 0.49 ± 0.09 mg/100 g for Cu; 1.6 ±0.2 mg/100 g for Zn. Both Pb and Cd were determined below the limit of detection （LOD 5 0.10 mg/100 g）. The LOD values were determined for each element. The TPC content in defatted samples was slightly lower than the non-defatted ones, showing the dependence on the sample preparation. The calculated average levels of the elements were compared with the maximum levels recommended or regulated by the national legislation.

Uncertainty Estimation for the Determination of Trace Heavy Metals in Human Hair by Flame and Electrothermal Atomic Absorption Spectrometry

Trace element analysis on hair samples has been widely used to assess wildlife and human exposure to different contaminants present in the environment or at the workplace. Pollutants due to the presence of toxic metals in environment not only enter the body by breading, water, and foodstuff accumulates in hair, but they could be adsorbed directly on the hair from environment. In order to remove adsorbed elements and thus determine the internally bound elements correctly, hair sample must be washed. In the present work, we propose uncertainty estimation for the analytical results that are obtained from determination of cadmium, lead, copper, iron, manganese and nickel in human hair by flame and electrothermal atomic absorption spectrometry （FAAS and ETAAS）. To estimate the uncertainty of analytical result obtained, two types of bias are calculated in the assessment of trueness： a proportional bias and a constant bias. Nested design was applied for calculating proportional bias and Youden method to calculate the constant bias. The results we obtained for proportional bias are calculated from spiked samples. In this case, the concentration found is plotted against the concentration added and the slop of standard addition curve is an estimate of the method recovery. Estimated method of average recovery in human hair is： （1.019 ±0.026）, （0.918 ±0.014）, （1.073±0.016）, （1.0597± 0.017）, （1.073± 0.020） and （0.934± 0.117） for Cd, Pb, Mn, Ni, Fe and Cu respectively.

Blood Lead Levels During Pregnancy and Its Influencing Factors in Nanjing,China

Objective To investigate the blood lead levels （BLLs） in the duration of pregnancy and 6-12 weeks after delivery, and analyze the influencing factors of BLLs in healthy pregnant women. Methods Pregnant women were recruited from September 2009 to February 2010 at the prenatal clinic in Nanjing Maternity and Child Health Care Hospital. Altogether 174 healthy pregnant women without pregnant or obstetric complications or abnormal pregnancy outcomes were enrolled as the gravida group, and 120 healthy non-pregnant women as the control group. BLLs during pregnancy were determined by flame atomic absorption spectroscopy. Results BLLs in all the three pregnancy trimesters and postpartum were 59.8±24.3, 55.4±20.1, 55.9±19.7, and 67.6±17.4 μ/L, respectively, and the mean BLL in control group was 67.5±21.3 μg/L. BLLs during all the three trimesters were lower in the gravida group than in the control group （P=0.043, 0.021, and 0.028）. Furthermore, occupations, nutrients supplementation, and time of house/apartment painted were associated with BLLs in pregnant women. Lead-related occupations, cosmetics use, and living in a house painted less than 1 year before are risk factors of high BLLs among pregnant women, while calcium, iron, zinc, and milk supplements are protective factors. Conclusion Supplementing calcium, iron, zinc, and milk, or avoiding contact with risk factors may help people, especially pregnant women, to reduce lead exposure.