液态分散系中丁达尔效应的研究和实验改进

针对以高单色、高亮度红色激光作光源,一般分散系都有光散射现象,难以区分胶体和溶液这一问题,用普通白色聚光小手电筒进行了对照实验,不仅很好地区分了胶体和溶液,而且排除了蓝色溶液吸收红光所产生的干扰,通过分析一般分散系产生光散射现象的条件,得出了利用丁达尔效应区分胶体和溶液应注意的问题。并把丁达尔效应实验从气溶胶、液溶胶、固溶胶3个角度进行改进,最终得到3个改进实验：巧做气溶胶丁达尔效应实验、利用固溶胶做丁达尔效应实验、建立实验盒模式做液溶胶丁达尔效应实验。改进后的实验具有装置简单、操作简便,现象明显、节能环保等优点。     

Study of The Thermal Decomposition of Some New Cyanine Dispersed Dyes

The structure of the studied compounds was confirmed by elemental analysis, IR and NMR. TG and DTG data were used to study the kinetics of the thermal decomposition process of some new cyanine dispersed dyes derived from 2-[(p-chloro)-styryl]-6-[5-(3-aryl-rhodanine)]-1,2-dihydropyridine. The reaction was found to follow first order mechanism. The activation energy E_a was calculated and used to calculate the thermodynamic parameters enthalpy change (H^*), entropy change (S^*), and free energy change (G^*), related to the thermal decomposition process. Two different calculation methods including Coats—Redfern and Chatterjee were applied to evaluate thekinetic and thermodynamic parameters. Quantum study was performed to support both the structure and the thermal data.This revised version was published online in November 2005 with corrections to the Cover Date.     

动物源性食品中四环素类残留分析研究进展

综述了检测动物源性食品中四环素类残留的前处理方法,包括固相萃取、固相微萃取、基质分散技术、分子印迹技术、限进介质材料;对高效液相色谱、毛细管电泳、微生物法和酶联免疫分析等在四环素类药物中的检测应用进行了综述,比较了各种方法的优缺点。     

高效液相色谱法测定保健食品中大豆异黄酮含量

建立了高效液相色谱法(HPLC)测定保健食品中大豆异黄酮含量的方法,运用二极管阵列检测器(PDA)建立了4种大豆异黄酮D、G、De、Ge的光谱库,测定了D、G、Ge与De响应值之比.采用PDA检测,C18反相柱,以甲醇∶水∶醋酸(HAC)=55∶45∶1(V/V/V)为流动相测定了同一批保健食品美龄营养片中4种大豆异黄酮D、G、De、Ge的含量分别为2.24%、10.82%0、.085%、0.027%,变异系数小于5%,回收率为92.51%～99.30%.该方法快速,精密度及准确度在允许范围内,可作为保健食品中D,G,De,Ge的同时测定方法.     

离子型食品的研制及其意义

介绍了离子型食品(包括:离子型食用钙和多元素食用离子粉)的研制及其意义。这些离子型食品能将不溶于水的矿物质转化为可溶于水的元素离子,以解决人体因胃酸不足对矿物质吸收利用差的问题,成为人体矿物质元素新的直接来源。基此可开发出系列离子型食品。     

Cleavage of C-S Bond of Sulfolane Induced by Ultrasonically Dispersed Potassium

The reductive cleavage of the carbon-sulfur bond of sulfolane has been reinvestigated; a reaction mechanism is proposed.     

Spectrofluorometric Determination of Thiamin and Riboflavin in Vegetable Foods

Abstract

Modifications of the AOAC thiamin and riboflavin methods allow effective and simple determination of both vitamins from aliquots of the digested sample of vegetable foods. Study of the minimum amount required for a complete hydrolysis of the vitamers corresponding to each vitamin have been carried out. A critical study of thiocrome formation which was later used in the spectrofluorimetric determination of thiamin was done. In order to separate riboflavin from the digested sample, a new liquid chromatographic method based on adsorption in florisil is proposed. The aforementionated methods were applied to different samples of several vegetable foods.     

离子色谱法测量休闲食品中的柠檬酸盐

建立了离子色谱法测定休闲食品中柠檬酸和柠檬酸盐含量的方法。采用标准曲线法定量,柠檬酸浓度在1.0~20.0 μg/mL的范围内,线性方程为y=0.049 9x-0.017 4,线性相关系数为0.998 2,方法的检出限为0.015 μg/mL,加标回收率为96.9%~101.6%,方法具有简单、快速、重现性好等优点。     

高效毛细管电泳法同时测定减肥类功能食品中7种违禁成分

建立了同时测定减肥类功能食品中违禁成分芬氟拉明、伪麻黄碱、去甲伪麻黄碱、安非拉酮、西布曲明、西地那非和士的宁的高效毛细管电泳分析方法。以20 mmol/L硼砂-10 mmol/L SDS-5%乙腈溶液(pH9.0)为运行缓冲液,在25℃,17 kV条件下测定,检测波长为195 nm。各待测物线性范围上限均为100 mg/L,线性相关系数均大于0.998,相对标准偏差为4.5%~7.9%(n=7);平均加标回收率为79.6%~112.0%;检出限(S/N=3)为0.16~0.65 mg/L。本方法简便快速、灵敏准确、分析成本低,已成功应用于功能食品中上述减肥类违禁添加成分的测定。     

全息聚合物分散液晶的结构调控与性能

全息聚合物分散液晶(HPDLCs)是由富聚合物相与富液晶相周期性排列而成的结构有序高分子复合材料.HPDLCs通过单体/液晶复合体系的光聚合诱导相分离而形成,如何调控并定量化描述复合体系的光聚合反应动力学、凝胶化行为和相分离程度,进而获得结构规整、电光性能优异的HPDLCs是关键难题.专论概述了光引发体系、单体结构、纳米无机材料掺杂对HPDLCs结构及性能的影响.光引发阻聚剂通过引发和阻聚的竞争与协同,降低了光聚合反应速率、延迟了凝胶时间,促进形成衍射效率达90%的HPDLCs.超支化单体降低了复合体系黏度和光聚合反应速率,延迟了凝胶时间,促使形成衍射效率达94%、具有一维光子晶体结构的HPDLCs.丙烯酰胺单体优化了相分离结构,将HPDLCs的衍射效率提升至98%.纳米硫化锌掺杂在保持规整结构和高衍射效率的同时,大幅降低了HPDLCs的驱动电压.研究还确定了HPDLCs的相分离程度与凝胶时间的函数关系.构建兼具高衍射效率与低驱动电压的HPDLCs,推进其在彩色3D图像存储等领域的应用仍是重要课题.     

毛细管电泳法快速测定保健食品中免疫球蛋白G

建立了毛细管电泳法快速测定保健食品中免疫球蛋白G(IgG)含量的方法,成功测定了不同剂型(片剂、粉剂及胶囊)牛初乳保健品中IgG的含量。以37 cm×50μm(i.d.)未涂敷熔融石英毛细管为色谱分离柱,50 mmol/L四硼酸钾 65 g/L聚乙二醇20 000(1 mol/L氢氧化铯调pH 10.0)为运行缓冲液,于214 nm波长处检测。详细研究了影响实际样品中IgG分离及准确定量的关键因素,如添加剂的种类、浓度;运行及样品缓冲液的浓度及pH等。采用峰面积外标法定量。方法的精密度为2.1%(n=7);检出限为6.25 mg/L(S/N=3);线性范围为50~2000 mg/L;400 mg/L IgG迁移时间的相对标准偏差(RSD)为0.14%;峰面积的RSD为2.9%(n=7)。6 m in内即可实现保健食品中IgG的分离与测定,结果与产品标示值基本吻合。     

气相色谱-质谱法测定油炸淀粉类食品中的丙烯酰胺

 建立了油炸淀粉类食品中丙烯酰胺的溴衍生化气相色谱-质谱(GC-MS)测定方法。样品经水提取、高速离心、石墨化 炭黑柱净化、溴衍生化后,以GC-MS选择离子进行定性,同位素稀释技术定量。该方法的检出限为5 μg/kg,回收率为90％ ～105％,相对标准偏差为6.3％。利用该方法对市场上某些油炸淀粉类食品进行了初步测定,发现薯片和炸薯条中含有27 8~4518 μg/kg的丙烯酰胺。     

Assessment of Lead and Cadmium in Canned Foods by Square-Wave Anodic Stripping Voltammetry

Abstract

This work reports the simultaneous determination of lead and cadmium in canned foods samples using square-wave anodic striping voltammetry (SWASV) on a bismuth film electrode (BiFE). The metal ions and bismuth were simultaneously deposited by reduction at ?1 V on a rotating carbon-paste disk electrode. Then, the preconcentrated metals were oxidized by scanning the potential of the electrode from ?1 to ?0.4 V using a square-wave waveform. The electrode displayed excellent linear behavior in the examined concentration range, from 5 to 150 µg/L of cadmium and lead (r² = 0.999 for both). Using the optimized conditions, the limits of detection were 0.27 µg/L for cadmium and 0.35 µg/L for lead. The reproducibility of the proposed sensor, evaluated in terms of relative standard deviation (RSD), were 5.8% and 3.7% of Cd and Pb, respectively for five measurements. Finally, the system based on BiFEs combined with rotating disk electrode was applied to determination of lead and cadmium in canned food samples. The results obtained were validated by inductively coupled plasma optical emission spectroscopy (ICP-OES).     

Determination of Vanadium in Foods by Atomic Absorption Spectrophotometry

ABSTRACT

A simple and sensitive method for the determination of vanadium in foods was established by using atomic absorption spectrophotometry with graphite furnace atomization. The proposed method includes formation of a chelate-complex by reacting vanadium with pyrrolidine dithiocarbamate (PDCA), extracting the chelate with xylene and measurement of the extract by atomic absorption. The recoveries of added vanadium to various foods were 91.3 and 109.1%, within 7.9% of the coefficient variation. The sensitivity of this method is 10 - 50 times higher than previous methods with a detection limit of 0.01 μg/g.     

聚合物分散液晶PMMA-5CB的制备及电光性能

以聚合引发相分离的方法制备了聚甲基丙烯酸甲酯(PMMA)基聚合物分散液晶(PDLC).通过差示量热扫描仪(DSC)、偏光显微镜(POM)对不同液晶5CB(4-氰基-4'-戊基联苯)含量的PDLC热力学行为和液晶分散状态进行了表征.在电压为0～30 V、波长为633 nm处,用紫外可见分光光度计(UV-Vis)对PDLC的电光性能进行了研究.结果表明当w(5CB)达到20%以上时,PDLC发生相分离现象;当w(5CB)=30%时,液晶的分散状态最佳,电光效应最强.     

Atomically Dispersed Single Co Sites in Zeolitic Imidazole Frameworks Promoting High-Efficiency Visible-Light-Driven Hydrogen Production

As photocatalysis technology could transform renewable and clean solar energy into green hydrogen (H₂) energy through solar water splitting, it is regarded as the “Holy Grail” in chemistry field in the 21st century. Unfortunately, the bottleneck of this technique still lies in the exploration of highly active, cost-effective, and robust photocatalysts. This work reports the design and synthesis of a novel zeolitic imidazole framework (ZIF) coupled Zn_0.8Cd_0.2S hetero-structured photocatalyst for high-performance visible-light-induced H₂ production. State-of-the-art characterizations and theoretical computations disclose that the interfacial electronic interaction between ZIF and Zn_0.8Cd_0.2S, the high distribution of Zn_0.8Cd_0.2S on ZIF, and the atomically dispersed coordinately unsaturated Co sites in ZIF synergistically arouse the significantly improved visible-light photocatalytic H₂ production performance.     

采用柠檬酸合成高分散铜催化剂用于选择氢解反应

A highly dispersed Cu catalyst supported on silica was prepared by an incipient wetness impregnation method with citric acid.The synthesis was studied by nitrogen physisorption,X-ray diffraction,and temperature-programmed reduction by comparing with a reference prepared without citric acid.The catalyst precursor obtained after impregnation was X-ray amorphous.The precursor was readily transformed to crystalline CuO upon calcination.The CuO particles were of uniform size in a highly dispersed state and can be reduced to Cu at a lower temperature.The activity of the Cu catalyst obtained was an order of magnitude higher than that of the reference for the hydrogenolysis of methyl laurate to dodecanol.     

Determination of Traces of Chromium in Foods by Solvent Extraction Flame Atomic Absorption Spectrometry

ABSTRACT

A simple methodology for Cr(III) determination in foods was developed through flame atomic absorption spectrometry with air/acetylene after a fast oxidation of Cr(III) with KM_nO₄ and pre-concentration of Cr(VI) in MIK as C_rO₂CI₂. A limit of detection and limit of quantification (LOQ), respectively, of 4 μg/Kg and 13 μg/Kg Cr(III) were obtained in commercialized foods in São Paulo, Brazil. Two certificated samples as well as some food samples were analyzed with good results. A study of sample treatment showed that the dry ash method is the best.