Effect of carbon-supported and unsupported Pt–Ru anodes on the performance of solid-polymer-electrolyte direct methanol fuel cells

The structure, chemistry and morphology of commercially available carbon-supported and unsupported Pt–Ru catalysts are investigated by X-ray diffraction, energy-dispersive analysis by X-rays and electron microscopy. The catalytic activities of these materials towards electrooxidation of methanol in solid-polymer-electrolyte direct methanol fuel cells have been investigated at 90C and 130C with varying amounts of Nafion ionomer in the catalytic layer. The unsupported Pt–Ru catalyst exhibits higher performance with lower activation-control and mass-polarization losses in relation to the carbon-supported catalyst.On leave from the     

固相萃取-气相色谱测定地下水中多环芳烃的质量控制研究

以USEPA及国家标准为基础研究了利用固相萃取——气相色谱测定地下水中16种多环芳烃的分析方法．探讨了几种空白用水的效果，得出市售纯净水是最简单且效果最好的空白溶剂，同时研究表明．该分析方法的检出限可以达到0．004～0．010μg／L．标准偏差在2．6％～12．4％范围内。基质加标回收率达到71．5％～99．7％。本研究方法不仅适用于地表水中多环芳烃的分析测定．同时也可以用于地下水及各种淋滤水样中多环芳烃的分析测定。为国内尽快建立利用固相萃取技术处理环境样品中多环芳烃的标准方法提供必要的数据依据。     

离子色谱法同时测定牛奶及其制品中的亚硝酸盐、硝酸盐、硫酸盐和硫氰酸盐

建立了离子色谱同时测定牛奶及其制品中亚硝酸盐、硝酸盐、硫酸盐和硫氰酸盐的方法.该方法采用三氯乙酸-乙醇对样品进行萃取并离心,上清液经C18固相萃取小柱净化后,利用阴离子色谱柱分离、检测.试验结果表明:该方法的线性范围和相关系数为0.02～5.0 μg/mL和0.9992,检出限为0.005～0.02 mg/kg;相对标...     

固相萃取-高效液相色谱法测定七种痕量生物胺

研究了固相萃取-高效液相色谱法测定痕量7种生物胺(色胺、酪胺、组胺、腐胺、尸胺、精脒、精胺)的方法。7种不同生物胺的标样混合溶液与荧光衍生剂丹酰氯在特定条件下衍生,衍生后通过C18固相萃取柱净化、富集,InertsilODS-3色谱柱分离,荧光检测器检测,流动相为乙腈和水梯度洗脱20min,流速为1mL/min。变异系数(CV%)为0.51～2.23,检测低限为1.29×10-6～2.57×10-4μg/mL。     

蔗糖多酯的合成研究进展

蔗糖多酯（SPE）是一种新兴的功能性食品添加剂,具有广阔的发展前景。它作为一种新的脂肪替代品,在不久的将来必定会在食品工业中得到大规模的推广和应用。本文综述了蔗糖多酯的营养保健功能、工业用途和合成方法的国内研究进展情况,提出了蔗糖多酯的开发设想。     

Optimised off-line SPE–GC–FID method for the determination of mineral oil saturated hydrocarbons (MOSH) in vegetable oils

An optimised off-line SPE–GC–FID method based on the use of silver-silica gel was developed for the determination of mineral oil saturated hydrocarbons (MOSH) in vegetable oils, including olive pomace oil. The method is specific in not including the aromatic hydrocarbons. The performance of different silica gels (untreated, activated and treated with silver nitrate) was compared in terms of capacity to retain fat and retention of interfering olefins present in particularly large amounts in refined olive oils. A coefficient of variation of 9% was obtained performing six replicate analyses of an extra virgin olive oil fortified with an amount of MOSH near the estimated LOQ (15 mg/kg). Recoveries were close to 100%. The use of activated aluminium oxide as an additional tool to eliminate interference by endogenous long-chain n-alkanes, is discussed.     

Solid state 27Al NMR and X-ray diffraction study of alumina–carbon composites

The structural and chemical transformations occurring in alumina–carbon composites upon heat treatment were investigated by using a combination of X-ray diffraction (XRD) and solid-state ²⁷Al nuclear magnetic resonance (NMR) spectroscopy. Two different carbon precursors were employed: a commercial activated carbon and a char obtained by carbonization of the endocarp of babassu coconut at 700 °C. The alumina–carbon composites were prepared by aqueous impregnation of the carbon supports with aluminum nitrate and, after filtering and drying, the as-synthesized powders were heat-treated under argon flow at temperatures up to 1000 °C. The Al compounds present in the as-synthesized samples were identified by XRD and solid-state ²⁷Al NMR as nanocrystalline aluminum oxyhydroxides or hydroxides, depending on the synthesis conditions. All Al-containing phases were XRD-amorphous in the char-derived nanocomposites, with the presence of a distribution of AlO₆ (octahedral Al site), AlO₅ (pentacoordinated Al) and AlO₄ (tetrahedral Al site) units revealed by solid-state ²⁷Al NMR spectroscopy. The heat treatments caused the formation of transition aluminas dispersed over the carbon supports, with the occurrence of different amounts of AlO₆, AlO₅ and AlO₄ units depending on the heat treatment temperature and on the type of carbon precursor used for the preparation of the composites.     

QuEChERS-HPLC法测定植物性食品中氟吗啉的残留量

以苹果、梨、葡萄、橘子、白菜、西兰花、菠菜、胡萝卜、番茄和黄瓜共10种植物性食品为研究对象,建立了植物性食品中氟吗啉残留量的QuEChERS-HPLC检测方法。样品经0.1%冰醋酸乙腈提取,醋酸钠和无水硫酸镁盐析后,取上清液,加入伯仲胺粉分散固相萃取净化,用配有二极管阵列检测器的高效液相色谱测定,外标法定量。氟吗啉在0.1~2mg/L的范围内具有较好的线性关系,氟吗啉在0.1、0.2、0.5mg/kg三个添加水平平均回收率81%～116%,RSD2.3%~12.1%,定量限为0.05mg/kg。本方法前处理简单、快速,适用于多种植物性食品中氟吗啉残留量测定。     

Optimization of ethanol extraction and further purification of isoflavones from soybean sprout cotyledon

Isoflavones from cotyledons of soybean sprouts were extracted with aqueous ethanol and further concentrated to obtain a product with a high concentration of isoflavone. The ethanol concentration, extraction time and reaction temperature were optimized by using response surface methodology (RSM). Isoflavones in aqueous ethanol were concentrated by a three-step procedure comprised of solid phase extraction (SPE) with Diaion HP-20 and Amberlite-XAD-2 adsorption columns, acid hydrolysis, and liquid–liquid extraction. The maximum amount of isoflavone in aqueous ethanol extracts (11.6 mg/g solid) was obtained when isoflavones in cotyledons (2.18 mg/ g solid) were extracted with 80–90% (v/v) aqueous ethanol above 90 °C for more than 100 min. The isoflavone extracts, obtained by SPE with a Diaion HP-20 column contained 100 mg/g solid. The liquid–liquid extraction (LLE) with ethyl ether further concentrated the extracts up to 229 mg/g solid, retaining 63% of the initial isoflavones.     

固相萃取—气相色谱法测定大豆粉中的有机磷

建立了一种快速测定大豆粉中有机磷农药残留的气相色谱法。试样中的农药残留用乙腈提取,提取液经氮气浓缩后用C18柱和Envi-Carb＋NH2串联柱净化,气相色谱—火焰光度检测器（FPD）测定。有机磷农药的加标回收率为92.6-105%,在0.1-4mg/kg内有比较好的线性关系,相关系数为0.999,方法的检出限为0.005mg/kg。该方法灵敏度、准确度和精密度均符合农药残留测定的技术要求。