Determination of bisphenol A in human breast milk by HPLC with column-switching and fluorescence detection

A highly sensitive HPLC method was developed for the determination of xenoestrogenic compound, bisphenol A (BPA) in human breast milk samples. After a two-step liquid-liquid extraction, BPA was derivatized with fluorescent labeling reagent, 4-(4,5-diphenyl-1H-imidazol-2-yl)benzoyl chloride (DIB-Cl). The excess fluorescent reagent could be removed effectively using a column-switching system. The separation of DIB-BPA from endogenous materials in milk was carried out on two C(18) columns and fluorescence intensity was monitored at 475 nm with the excitation of 350 nm. A good linearity (r = 0.994) was observed of BPA in the concentration range of 0.2-5.0 ng mL(-1) in breast milk, and the detection limit was 0.11 ng mL(-1) at a signal-to-noise ratio of 3. Intra- and inter-day precision (RSD, %) were less than 8.7 and 10.4, respectively. Twenty-three breast milk samples of healthy lactating women were analyzed for the BPA concentration; the mean value was 0.61 +/- 0.20 ng mL(-1), with no correlation to the lipid content of milk samples.     

The mixed valent tellurate SrTe3O8: Electronic lone pair effect of Te

A novel mixed valent tellurium oxide, SrTe₃O₈, has been synthesized and its crystal structure was determined ab initio from powder X-ray diffraction data. This oxide, which crystallizes in a tetragonal unit-cell, P4₂/m space group, with very close a and c cell parameters (6.8257(1) and 6.7603(1) Å, respectively), exhibits a very original structure built up of corner-sharing TeO₆ (Te⁶⁺) octahedra and Te₂O₈ (Te⁴⁺) twin-pyramidal units. The latter ones form [Te₃O₈]_∞ chains running along the [001] and the [110] directions. Besides the four sided tunnels where the Sr²⁺ cations are located, there are very large four sided tunnels running along the c-axis which are obstructed by the electronic lone pairs of the Te⁴⁺ cations.     

Multi-element characterization of silicon nitride powders by atomic and mass spectrometric solution methods

A sample pretreatment technique for silicon nitride involving digestion and matrix/traces separation was developed by means of radiotracers and applied to analysis of this material by inductively coupled plasma atomic emission spectrometry, inductively coupled plasma mass spectrometry and graphite furnace atomic absorption spectrometry. The results obtained for a high purity silicon nitride material by these methods are compared each with the other and with those obtained by neutron activation analysis. The limits of detection and the capabilities of the methods are compared and discussed.     

Bifonazole-β-cyclodextrin Inclusion Complexes. Thermal analysis and X-ray powder diffraction study

The complexation of bifonazole, an antimycotic hydrophobic imidazole derivative, with β-cyclodextrin (β-CD) was investigated in solid phase, using the following complementary techniques: differential scanning calorimetry (DSC), thermogravimetric analysis (TG) and X-ray powder diffractometry. The β-CD-bifonazole samples were prepared in both aqueous medium by coprecipitation and in solid state by kneading method and the β-CD-bifonazole binary diagrams were drawn. The experimental results demonstrate the formation of two binary compounds, β-CD-bifonazole and (β-CD)_x bifonazole (x =2 or 4). The first compound may be an inclusion compound and the second a crystallized compound, in which the bifonazole is not necessarily included in the cyclodextrin internal cavity. This revised version was published online in July 2006 with corrections to the Cover Date.     

H2S-sensing properties of SnO2 produced by ball milling and different chemical reactions

In this work, the mechanochemical synthesis of a moderately agglomerated tin oxide (SnO₂) powders and the subsequent preparation of semiconductor gas sensors as prototypes, were studied. Tin (II) chloride (SnCl₂) powder was milled with calcium hydroxide (Ca(OH)₂) and potassium carbonate, (K₂CO₃) powder, respectively, in a ball mill at room temperature and in an air atmosphere. Heat treatment of milled mixtures at 400 °C resulted in the formation of a tetragonal phase, confirmed by X-ray diffraction (XRD). During milling in the presence of water, a high number of hydroxide (OH) groups are formed at the surface. When SnCl₂ was milled with K₂CO₃, no water was produced and the Fourier-transform infrared spectrum (FT-IR) of the powder has no surface hydroxyl deformations. On exposure to hydrogen sulfide (H₂S) gas, the particles, prepared from anhydrous powder, have higher sensitivity than these, prepared from hydrated powder. The SnO₂ thick film, prepared from anhydrous powder may be successfully applied to a H₂S gas sensor.     

改进的微波辅助无溶剂法提取薄荷和陈皮中的挥发油组分

An improved solvent free microwave extraction, in which a kind of microwave absorption medium （carbonyl iron powder） was used, was applied to the extraction of essential oil from dried menthol mint and orange peel without addition of any solvent and pretreatment. It took much less time of extraction （30 min） than microwave-assisted hydrodistillation （90 min） and conventional hydrodistillation （180 min）. The kinds of chemical compositions in essential oil extracted by different methods were almost the same and such improved solvent free microwave extraction can be a feasible way in extraction of essential oil from dried plant materials.     

Structural disorder in Ba0.6Sr0.4Al2O4

The structural disorder in Ba_0.6Sr_0.4Al₂O₄ (space group P6₃22) was investigated by X-ray powder diffraction and selected-area electron diffraction (SAED). The initial structural model was determined using direct methods, and it was further modified by the combined use of Rietveld method and maximum-entropy method (MEM). MEM-based pattern fitting method was subsequently applied, resulting in the final reliability indices of R_wp=9.61%, R_p=6.96%, R_B=1.40% and S=1.25. The electron density distribution was satisfactorily expressed by the split-atom model in which the strontium/barium and oxygen atoms were split to occupy the lower symmetry sites. The diffuse scattering in SAED was mainly attributable to the positional disorder of oxygen atoms.     

Thermal stability and degradation of the post-use reclaim milk pouches during multiple extrusion cycles

In the present study, the recyclability of the post-use milk pouches (50/50 LDPE–LLDPE blend) was evaluated with or without adding stabilizer. Thoroughly washed and dried post-use milk pouch films were extruded five times at high temperature (483–513 K) in the open atmosphere. The mode of degradation during extrusion operation was studied by melt flow index (MFI), rheological properties, gel content and FT-IR analysis. The differential scanning calorimetry (DSC) analysis was carried out to evaluate the thermal stability of the stabilized and un-stabilized recycled mass from post-use milk pouch under this investigation. Mechanical properties (tensile strength, % elongation at break, tensile modulus and hardness) of the un-stabilized extruded material were significantly affected as a result of thermooxidative degradation during extrusion in presence of air. After all, stabilization with 0.4% anti-oxidant satisfactorily retains all the initial properties of the recycled material.     

锂离子电池正极材料LiMn2O4的低热固相合成与性能表征

锂离子电池具有比能量高、环境污染小等优点,广泛应用于手提电话、便携式电脑、摄像机等设备中。其正极材料的研究是锂离子电池的研究重点。层状结构的LiCoO2、LiNiO2和尖晶石结构的LiMn2O4是仅有的三种能在3.5V以上电位可嵌入Li的正极材料[1~3]。目前市售的锂离子电池主要采用LiCoO2作正极材料,但由于Co资源缺乏和价格相对昂贵,而锰资源丰富,价格低廉且无毒,对环境友好,因此世界各国都在大力进行以LiMn2O4为正极材料的锂离子电池的实用化研究。LiMn2O4传统的制备方法是高温固相反应合成法[4~7],但由于Mn的变价多,与Li形成贫Li或…     

Comparison of two methods for the extraction of fat from human milk

We compared two methods for the extraction of fat from human milk. Pure fat extraction techniques are necessary for qualitative and quantitative analysis of milk fat, of which triglycerides account for more than 98%. Method I was a conventional liquid-liquid system for the fat extraction while method II was a faster approach using a haematocrit technique. No significant differences were observed between both methods neither in the fat content determined gravimetrically, nor in qualitative and quantitative analysis of triglycerides by high-performance liquid chromatography (HPLC) with evaporative light-scattering detection (ELSD). We conclude that method II offers substantial advantages over the conventional method (method I). The former requires less reagents and material and is simpler and less time-consuming (approximately 30 min instead of 90 min). Therefore, a new method will make it possible to extract fat of more human milk in the same time.