Minor and Trace Element Analysis in Breast Milk Using Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

 Thirty-two breast milk samples provided voluntarily by healthy women living in the Dongting Lake area were investigated by Inductively Coupled Plasma Mass Spectrometry (ICP/MS). Eleven minor and trace elements (Na, Mg, K, Ca, Mn, Fe, Cu, Zn, As, Se and Pb) were quantified and compared with literature reports. The results provide useful data for further studies in the nutritional field. Author for correspondence. E-mail: zhengmh@mail. rcees.ac.cn Received September 4, 2002; accepted February 11, 2003 Published online May 15, 2003     

Comparison of original and modified BCR sequential extraction procedures for the fractionation of copper, iron, lead, manganese and zinc in soils and sediments

This article describes a detailed comparison between the original BCR sequential extraction procedure, step 2 of which involves treatment with 0.1 mol l⁻¹ hydroxylammonium chloride at pH 2, and the revised BCR procedure (step 2: 0.5 mol l⁻¹ hydroxylammonium chloride at pH 1.5). An intermediate protocol was also evaluated in which 0.5 mol l⁻¹ hydroxylammonium chloride at pH 2 was used. The procedures were applied to five soil and sediment substrates: a sewage sludge-amended soil, two different industrially contaminated soils, a river sediment and an inter-tidal sediment. Extractable iron and manganese concentrations were measured to assess the effects of the procedural modifications on dissolution of the reducible matrix components. Trace elements copper, lead and zinc were also determined. Statistical analysis (two-tailed t-tests at 95% confidence interval) indicated that recovery of iron in step 2 was not markedly enhanced when the intermediate protocol was used. However, significantly greater amounts were isolated with the revised BCR scheme than with the original procedure. Copper behaved similarly to iron. Lead recoveries were increased by use of both modified protocols, with the greatest effect occurring for the revised BCR extraction. In contrast, manganese and zinc extraction did not vary markedly between procedures. The work indicates that the revised BCR sequential extraction provides better attack on the iron-based components of the reducible matrix for a wide range of soils and sediments.     

Determination of Nitrogen in Duplex Stainless Steels by EPMA

 We describe the quantitative determination of low nitrogen contents (< 1 %wt) in highly-alloyed, duplex stainless steels by EPMA using a calibration curve. Five monophasic stainless steels with various nitrogen concentrations were used for the calibration curve, namely, three highly alloyed steels prepared in the laboratory, with nitrogen contents 0.066, 0.565 and 1.016 %wt and two industrial alloys with nitrogen concentrations 0.174 %wt and 0.023 %wt. For these samples, the plot of nitrogen X-ray intensities versus nitrogen contents exhibited an acceptable linear relationship. Average nitrogen contents of the analysed duplex alloys were found to vary in the range < 0.045–0.07 %wt in ferrite and 0.52–0.77 %wt in austenite. These results suggest that the nitrogen solubility limit in ferrite has been reached; on the other hand, nitrogen solubility in austenite increases due to the high manganese and low nickel contents.     

A journey through the hazards of possible errors in the analysis of trace elements in body fluids and tissues

Accuracy of the analysis results of trace elements in body fluids and tissues needs to be ascertained during every step of the procedure, starting with the choice of sample, followed by appropriate sampling, analytical methodology and quality assurance, to end with the evaluation of the data. The characterisation of the reference group is important because it is fundamental in the decision making step. Appropriate sampling ensures that the concentration of the trace element in the collected sample is exactly the same as was originally present in the individual. Besides, sample manipulation should not alter the concentrations. The analytical technique chosen is supposed to offer sufficient specificity and sensitivity, and to allow the determination of the trace element with a signal exceeding the quantification limit of detection. Quality assurance through the analysis of similar levels in certified reference materials is a very valuable asset to prove the validity of the detection and to eliminate possible errors which may jeopardize the accuracy and reliability of the data.     

Application of an on-line preconcentration system in simultaneous ICP-AES

A PC-controlled on-line preconcentration system (TRACECON) developed by Knapp et al. [11], was connected to a JY-70 Plus simultaneous ICP spectrometer to preconcentrate on-line seven trace elements (Cu, Fe, Zn, Cr, Ni, Mn, V) in biological and environmental samples. EDTrA-cellulose was used as column material. The elemental concentrations were determined by simultaneous ICP-AES. The effect of pH of the sample solution on the enrichment was studied. It was found that the recoveries of chromium and iron depend strongly on the pH of the sample solution. All the elements mentioned were recovered quantitatively at pH 4.0±0.1. The flow rates of sample solution and element solution were optimized. The enrichment factors for seven elements at 5 ml loading volume range from 3.9 for Cu to 7.9 for Zn. The detection limits of all seven elements were improved. The accuracy of the method was tested by the analysis of a number of CRMs of NIST, BCR and NIES. Most results are in good agreement with the certified values.On leave from Shanghai Institute of Metallurgy, Academia Sinica, Shanghai 200050, People's Republic of China     

ICP-AES法测定盱眙野马追的微量元素

研究了用电感耦合等离子体原子发射光谱(ICP—AES)同时测定野马追全草和花蕾中微量元素的方法。采用干法和湿法消解：干法是先将样品600％高温灰化，再用浓硝酸溶解；湿法是用HNO3-HCIO4直接消解。结果表明，盱眙野马追中含有Fe、Al、Si等多种微量元素，其中Fe、Cu、Mn、Zn、Sr、Ni、Cr等是人体必需微量元素。对干法和湿法的测定结果进行了比较，得出用ICP-AES法测定野马追中的微量元素具有简单、快速、准确度高的优点。     

传统藏药材波棱瓜的微量元素分析

对传统藏药材波棱瓜中12种微量元素进行了分析。结果显示，在波棱瓜中人体必需微量元素Cu、Fe、Zn、Mn、Co、Ni、Cr、Se等含量较高；对西藏地区不同产地的波棱瓜中的微量元素含量作比较，有极显著差异。提示在选用药材时，应重视其产地。     

Organically modified silica gel and flame atomic absorption spectrometry: employment for separation and preconcentration of nine trace heavy metals for their determination in natural aqueous systems

A 5-formyl-3-(1′-carboxyphenylazo) salicylic acid-bonded silica gel (FCPASASG) chelating adsorbent was synthesized according to a very simple and rapid one step reaction between aminopropyl silica gel (APSG) and 5-formyl-3-(1′-carboxyphenylazo) salicylic acid (FCPASA) and its adsorption characteristics were studied in details. Nine trace metals viz.: Cd(II), Zn(II), Fe(III), Cu(II), Pb(II), Mn(II), Cr(III), Co(II) and Ni(II) can be quantitatively adsorbed by the adsorbent from natural aqueous systems at pH 7.0–8.0. The adsorbed metal ions can be readily desorbed with 1 M HNO₃ or 0.05 M Na₂EDTA. The distribution coefficient, K_d and the percentage concentration of the investigated metal ions on the adsorbent at equilibrium, C_M,_eqm % (Recovery, R%) were studied as a function of experimental parameters. The logarithmic values of the distribution coefficient, logK_d, are 3.7–6.4. Some foreign ions caused little interference in the preconcentration and determination of the investigated nine metals by flame atomic absorption spectrometry (AAS).The adsorption capacity of FCPASASG was 0.32–0.43 meq g⁻¹. C and N elemental analyses of the adsorbent (FCPASASG) allowed us to calculate a surface converge of 0.82 mmol g⁻¹. This value compares well with the best values reported for the azo compounds. The adsorbent and its formed metal chelates were characterized by IR (absorbance and/or reflectance) and UV spectrometry, potentiometric titrations and thermogravimetric analysis (TGA and DTG). The mode of chelation between the FCPASASG adsorbent and the investigated metal ions is proposed to be due to reaction of those metal ions with the salicylic and/or the carboxyphenylazo chelation centers of the FCPASASG adsorbent. Nanogram concentrations (0.07–0.14 ng ml⁻¹) of Cd(II), Zn(II), Fe(III), Pb(II), Cr(III), Mn(II), Cu(II), Co(II) and Ni(II) can be determined reliably with a preconcentration factor of 100.     

非典型肺炎与微量元素

论证了非典型肺炎合并病毒性心肌炎的可能性，提出其出现与亚健康和缺乏硒、锌、锰等微量元素有关。     

东莞市城区儿童血锌、铁、钙元素与饮食习惯、生长发育关系的研究

探讨了莞城地区幼儿园3～7岁儿童血锌、铁、钙值与饮食习惯、身高、体重、易感染情况的关系，以便进一步指导喂养。采用群体自愿参加者取静脉血，检测了血清锌、铁、钙。检测前向家长发问卷调查饮食习惯、易感染情况。抽血后测量身高、体重。结果表明，在城区7所幼儿园1125例受检儿童中，检出血锌、铁、钙异常者831例(73．9％)，其中低于正常值者525例(63．2％)。有不良饮食习惯儿童342例(30．4％)。有轻度营养不良189例(16．8％)。身高不达标342例(30．4％)。复感儿508例(54．8％)。结论为：(1)本组儿童低血锌情况严重，而血锌值与饮食习惯、易感染情况、身高有密切关系。(2)未发现一例低血清铁者。(3)儿童低血钙者较少，低血钙与不良饮食习惯有关。