金银花茶中8种微量元素溶出特性研究

目的 探究金银花茶样品中8种微量元素的溶出特性。方法 基于电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry,ICP-MS),测定样品中Na、Ca、Mg、Mn、Fe、Zn、Cu、Se 8种微量元素含量,并分别研究了浸泡时间、浸泡次数及浸泡温度与元素溶出特性之间的关系。结果 结果表明,金银花茶中微量元素含量丰富,8种元素含量由高到低的顺序为：Ca>Mg> Fe>Na>Mn> Zn>Cu>Se。各元素溶出量随浸泡时间延长而升高,其中Fe溶出率最低,表明Fe最难溶出。除Na和Se以外,各元素溶出量随浸泡次数增加而降低,随浸泡温度升高而升高;Na的溶出量随浸泡次数增加呈先降低后升高的趋势,而Se的溶出量随浸泡次数增加而降低;Na和Se的溶出量均随浸泡温度升高呈先升高再降低的趋势。各元素溶出量与浸泡时间、浸泡次数及浸泡温度之间的关系均可通过建立不同类型的数学模型进行描述。结论 从保健茶饮的功能性和风味角度考虑,金银花茶冲泡应选用100℃的水温,且冲泡次数应不超过4次。     

茶叶中重金属浸出规律的研究

采用火焰原子吸收光谱法测定了红茶和绿茶中铅、铜、锌的含量。考察了浸泡次数、浸泡温度和浸泡时间对铅、铜、锌3种金属元素浸出率的影响。结果表明,茶叶中铅、铜、锌的浸出率随浸泡次数的增多而减少,随浸泡温度的升高而增大,30min前随浸泡时间延长而增加。     

银杏茶中总黄酮的水溶浸出行为研究

以芦丁为标准品，采用分光光度法，以Al（NO3）3-NaNO2为显色剂，测定了市售银杏茶中总黄酮的含量，并考察了银杏茶在水中浸泡时浸泡温度、浸泡时间、浸泡次数、浸泡溶液的pH值等条件对银杏茶中总黄酮浸出的影响。结果表明，银杏茶中黄酮在水中浸出量受浸泡温度和浸泡溶液DH值的影响比较大。泡茶的溶液应避免使用酸性溶液。还对银杏茶的加工工艺进行了考察研究，发现银杏叶通过微波处理后，其黄酮的浸出量明显高出烘箱烘干的银杏叶的黄酮浸出量。因此，建议在银杏茶的加工工艺中采用微波干燥处理银杏叶。     

食品包装材料中双酚A在食品模拟物中迁移规律的研究

食品塑料包装材料的安全是保障食品安全的重要一环,包装材料中的双酚A潜在迁移性对人体健康的危害已引起社会的关注. 分别选取蒸馏水、3%乙酸(体积分数)和10%乙醇(体积分数)3种食品模拟物,浸泡已知双酚A含量的食品包装材料,在一定的时间点测试浸泡液中双酚A含量,研究迁移量与模拟物之间的关系. 结果表明,在不同食品模拟物下包装材料中双酚A的迁移量不同,其特定迁移量顺序为10%乙醇溶液>3 %乙酸溶液>蒸馏水. 并研究了温度、时间及微波作用影响食品包装材料中双酚A向食品中的迁移量,结果表明,双酚A向食品中迁移量随接触时间的延长、温度的升高而增加,微波作用能显著提高包装材料中双酚A向食品中的迁移量.     

自来水用橡胶软管中铅的析出分析

研究生活饮用水用橡胶软管中铅析出规律,选择3款橡胶软管,测定铅含量,并在自来水中分析不同浸泡时间以及普通浸泡温度(22、40、60、80、100℃)条件下铅析出量。结果表明,橡胶软管3#、1#、2#的铅含量依次降低,相同条件下铅析出量也依次降低;同一样品随着浸泡次数的增加,铅析出量呈现下降趋势;随着温度的升高,铅析出量呈现增加趋势,析出速率也在增加,铅含量高的橡胶软管铅析出量也高,铅析出量随着浸泡次数的增加而逐渐降低,随着浸泡温度的提高而增高。     

聚酯类食品包装材料中二氧化钛在食品模拟物中的迁移规律

采用电感耦合等离子体质谱法(ICP–MS),在不同的模拟迁移条件(模拟物、盛放温度、接触时间、乙酸浓度、使用次数等)下,研究聚酯类食品包装材料中二氧化钛在6种食品模拟物(水、4%乙酸、10%乙醇、65%乙醇、正己烷和异辛烷)中的迁移规律。结果显示:食品模拟物的属性对迁移行为有显著影响,迁移量随温度的升高及时间的延长而增加,食品的酸性越强,二氧化钛的迁移量越大。因此需适量控制聚酯类食品包装材料的反复使用次数、盛放食品时的温度和时间以降低二氧化钛迁出风险。     

6061铝合金微弧氧化陶瓷层生长速度的研究

以变形铝合金6061为试验材料,采用MAO240／750微弧氧化设备、TT260测厚仪和JSM6460扫描电子显微镜,研究了电流密度、占空比、样品尺寸和溶液温度等因素对铝合金微弧氧化陶瓷层生长速度的影响。结果表明：陶瓷层厚度随着时间的延长而线性增大,电流密度越大,陶瓷层生长速度越快,在相同时间内样品表面所达到的电压越高,电压的升高提高了陶瓷层被击穿继续发生内部氧化的能力;占空比大小对陶瓷层生长速度几乎无影响,而电压随着占空比的减小发生微小的上升;恒流氧化时,虽然陶瓷层的生长速度不随样品尺寸变化,但是电压随样品尺寸增大而升高;随着溶液温度的升高,溶液的导电能力增强,陶瓷层的生长速度变快。     

橡胶软管在自来水中铅析出分析

目的 研究生活饮用水用橡胶软管中铅析出规律。方法 选择3款橡胶软管,测定铅含量,并在自来水中分析不同浸泡时间以及不通浸泡温度(22、40、60、80、100 ℃)条件下铅析出量。结果 橡胶软管3_^#、1_^#、2_^#的铅含量依次降低,相同条件下铅析出量也依次降低;同一样品随着浸泡次数的增加,铅析出量呈现下降趋势;随着温度的升高,铅析出量呈现增加趋势,析出速率也在增加。结论 铅含量高的橡胶软管铅析出量也高,铅析出量随着浸泡次数的增加而逐渐降低,随着浸泡温度的提高而增高。     

高效液相色谱-串联质谱测定塑料聚合物中有机磷阻燃剂DOPO的迁移量及其迁移规律研究

采用高效液相色谱-串联质谱(HPLC-MS/MS)技术建立了塑料聚合物中9,10-二氢-9-氧-10-磷杂菲-10-氧化物(DOPO)迁移量的测定方法,并对不同浸泡模拟物、不同温度和时间下DOPO的迁移规律进行研究。样品采用欧盟(EU)2017/752法规中的食品模拟物浸泡。水基模拟物直接过滤,橄榄油模拟物用含38%甲醇的乙腈溶液萃取后,经C_(18)色谱柱分离,以甲醇-2 mmol/L醋酸铵水溶液(含0.1%甲酸)为流动相,采用多反应监测模式进行检测。水基模拟物(3%乙酸、10%乙醇、50%乙醇)中DOPO的定量下限为0.10 ng/mL,橄榄油模拟物中的定量下限为1.0 ng/g。样品加标回收率为85.3%～110%,相对标准偏差(RSD,n=6)不大于7.3%。该方法快速简便、灵敏度高、准确性好,适用于塑料聚合物中DOPO迁移量的测定。     

高效液相色谱法测定蜜胺-甲醛制品中三聚氰胺的特定迁移量

建立了高效液相色谱检测蜜胺-甲醛制食品接触材料和制品中三聚氰胺特定迁移量的分析方法。采用氨基柱分离样品,乙腈和水为流动相,检测波长为214 nm。方法的检出限是0.025μg/mL,线性范围是0.05~200μg/mL(r=0.9998),回收率为87.8%~95.1%,相对标准偏差小于1%,能够满足2009年9月1日即将实施的新的国家标准GB 9690-2009《食品容器、包装材料用三聚氰胺-甲醛成型品卫生标准》对三聚氰胺特定迁移量的限量(1.0 mg/kg)要求。该方法已应用于出口蜜胺-甲醛制品中三聚氰胺特定迁移量的检测。     

Sonochemical Processes and Formation of Gold Nanoparticles within Pores of Mesoporous Silica

Mesoporous silica with gold nanoparticles inside its pores was prepared by the soaking and ultrasound-induced reduction method. This new composite was characterized by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), and high-resolution transmission electron microscopy (HRTEM) techniques. The results showed that nearly spherical-shaped gold nanoparticles, with mean size in diameter of 5.2 nm, are located in the pores, most of which are less than 6 nm in diameter. The ultrasonic irradiation time dependence of optical absorption for the soaked porous solid sample, as suggested by the variation in absorbance at 310 and 544 nm, indicated the reduction of Au (III) ions, and the nucleation and aggregation of gold nanoparticles within pores of mesoporous silica. Additionally, the reaction rates estimated phenomenologically by the absorbance decay at 310 nm for both the porous sample and the corresponding soaking solution presented the enhancement of the sonochemical reduction rate of Au (III) ions within pores of mesoporous silica. It is assumed that the extensive liquid-solid interfacial zones in the pores, due to the high specific surface areas and great porosity of the mesoporous solid, are the major regions where the efficient sonochemical reduction induced by the cavitation takes place. Copyright 2001 Academic Press.     

Green dispersive solid-phase microextraction of melamine using crosslinked beta-cyclodextrin with citric acid followed by high-performance liquid chromatography

In this research, a green approach for dispersive solid phase microextraction was introduced for the extraction and determination of melamine in various matrices such as infant formula and hot water in a melamine bowl. In this way, a natural polar polymer called ß-cyclodextrin has been cross-linked with citric acid to create a water-insoluble adsorbent. The extraction was carried out by dispersion of the sorbent into the sample solution. The effective parameters on the extraction efficiency of the melamine, including ion strength, extraction time, sample volume, amount of absorbent, pH, type of desorption solvent, desorption time, and desorption solvent volume were optimized by one variable at a time approach. Under the optimal conditions, the method showed a good linear dynamic range for melamine in the range of 1–1000 μg/L with a coefficient of determination of 0.9985. The obtained limit of detection was 0.3 μg/L. The intra-day and inter-day relative standard deviations (n = 3) were 3.1% and 3.2% respectively. Lastly, this technique was applied to extract and determine the analyte in a melamine bowl and infant formula with acceptable and satisfactory results.     

液相色谱-串联质谱联用法测定食品中三聚氰胺残留量

提出了液相色谱-串联质谱联用法测定动物源性食品中三聚氰胺残留量的方法。样品采用乙腈进行提取,饱和氯化钠溶液进行分配经反相色谱分离后,串联质谱法进行测定,同位素内标法进行定量,方法的测定下限(10S/N)为0.05 mg·kg~(-1),以5类食品样品为基体,加入4种不同浓度水平的三聚氰胺标准作回收试验,测得回收率在72.9$～104.1%之间,测定值的相对标准偏差(n=6)在4.7%～15.2%之间。     

基于场放大进样和石墨烯量子点双重富集毛细管电泳分离检测三聚氰胺和双氰胺

通过热解法制备了硫掺杂的石墨烯量子点(S-GQDs),同石墨烯量子点(GQDs)相比,S原子的引入有效改善了GQDs的表面状态和化学特性、增强其对正电荷的捕获能力,使其更易与阳离子相互作用.以S-GQDs为载体,结合电堆积富集技术,发展了一种基于场放大进样(FASI)和S-GQDs放大的双重富集毛细管电泳(CE)分离检...     

Preparation of Hot Water-Resistant Silica Thin Films from Polysilazane Solution at Room Temperature

Perhydropolysilazane (PHPS) films were deposited on single-crystal Si substrates by spin-coating using a xylene solution of PHPS, and then suspended over 1 mol L^?1 ammonia water at room temperature. The PHPS-to-silica conversion occurring on the exposure to the ammonia water vapor was studied by infrared absorption spectroscopy. Si--H and N--H infrared absorption peaks decreased and Si--O--Si bands increased, showing PHPS-to-silica conversion; the conversion was almost completed in 6 h. The exposed films were soaked in 80°C water for 24 h, and the reduction in thickness on soaking was evaluated. The PHPS-derived films suspended over the ammonia water for 6 h exhibited only 2% reduction in thickness on soaking in 80°C water. Alkoxide-derived silica gel films dried in the ambient atmosphere or suspended over the ammonia water, on the other hand, exhibited significant reduction in thickness on soaking in 80°C water.     

高效液相色谱法测定禽蛋及其制品中的三聚氰胺

建立了高效液相色谱测定禽蛋类及加工品中三聚氰胺的检测方法．以经三聚氰胺标准添加的鸡蛋、咸鸭蛋和松花蛋为代表性样品,优化了提取溶剂的种类、用量和提取时间条件,探讨了直接过滤、正己烷反萃和固相萃取三种前处理方式的净化效果,并考察了测定时流动相比例和缓冲液的pH条件．实验结果表明：当添加浓度为0．20和10．0μg／g时,三聚氰胺的回收率分别为87．6％-101．5％,测量标准偏差为1．6％～2．8％,方法检出限为0．05μg／g．标准溶液在0．10～2．00μg／mL范围内,线性关系良好,相关系数r=0．9999．利用本方法对12个实际禽蛋样品进行测定,结果表明能够满足禽蛋及其制品中三聚氰胺残留的快速筛查要求．     

Effect of Soaking Conditions and Fuzzy Analytical Method for Producing the Quick-Cooking Black Jasmine Rice

The quick-cooking rice product is an interesting product for the market which is easy to cook, with good sensorial qualities and health benefits. This work aimed to study the effect of the soaking conditions, namely baking powder concentration (0.1, 0.2, or 0.3%), soaking temperature (room temperature, 50 or 60 °C), and soaking time (10, 20, or 30 min), in order to improve the physical properties and also the sensory characteristics, with high bioactive compound content, of Quick-Cooking Black Jasmine Rice (QBJR). The physical properties of the final product, namely the rehydration capacity, morphology, and texture, were observed. Moreover, the total phenolic, total flavonoid, and total anthocyanin were determined. The results showed that the samples with a high baking powder concentrations soaked at high temperatures for longer time affect the low rehydration capacity with a high hardness value and a decreased bioactive compound content. In addition, the sensory score including softener, flavor, and overall acceptance were lower score. Moreover, to determine the best soaking condition with complex data, the Fuzzy Analytical Method (FAM) was performed by an online FAM program. The results showed that soaking at room temperature for 30 min in 0.1% of baking powder showed the highest overall performance index of 6.52.     

铜质水嘴中铅含量与析出量的相关性探讨

试验探讨铜质水嘴中铅含量与析出量的关系。对一系列含铅标准铜片按照GB/T 17219–1998《生活饮用水输配水设备及防护材料的安全性评价标准》要求进行浸泡试验,使用原子吸收光谱法或电感耦合等离子体质谱法检测浸泡液中的铅含量,再利用20个已知铅含量的铜质水嘴样品进行析出量的检测和验证。得到铜质水嘴中铅含量与析出量的关系。试验结果表明:大部分内腔有电镀层的铜质水嘴,铅析出量小于5.0μg/L;内腔无电镀层的铜质水嘴中铅含量小于0.5%时,铅析出量小于5.0μg/L,符合GB/T 17219–1998标准要求。     

Robust Synthesis of Gold‐Based Multishell Structures as Plasmonic Catalysts for Selective Hydrogenation of 4‐Nitrostyrene

A robust self‐template strategy is used for facile and large‐scale synthesis of porous multishell gold with controllable shell number, sphere size, and in situ surface modification. The process involved the rapid reduction of novel Au‐melamine colloidal templates with a great amount of NaBH₄ in presence of poly(sodium‐p‐styrenesulfonate) (PSS). After soaking the templates in other metal salt solution, the obtained bimetallic templates could also be generally converted into bimetallic multishell structures by same reduction process. In the hydrogenation of 4‐nitrostyrene using NH₃BH₃ as a reducing agent, the porous triple‐shell Au with surface modification (S‐PTSAu) exhibited excellent selectivity (97 %) for 4‐aminostyrene in contrast with unmodified triple‐shell Au. Furthermore, it also showed higher enhancement of catalytic activity under irradiation of visible light as compared to similar catalysts with fewer shells.     

Preparation of a magnetic molecularly imprinted polymer with pseudo template for rapid simultaneous determination of cyromazine and melamine in bio-matrix samples

A magnetic molecularly imprinted polymer (M-MIP) for cyromazine and melamine was prepared by simple suspension polymerization using a pseudo template, 2-(4,6-diamino-1,3,5-triazin-2-ylamino)ethanethiol disulfide. The M-MIP was characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, and vibrating sample magnetometry. Molecular recognition properties and binding capability to cyromazine and melamine were evaluated by adsorption testing, which showed the M-MIP had better affinity and selectivity than the magnetic non-imprinted polymer (M-NIP) for cyromazine and melamine. A method based on molecularly imprinted solid-phase extraction assisted by magnetic separation was developed for extraction of cyromazine and melamine from bio-matrix samples. Various conditions, for example desorption conditions, amount of M-MIP, extraction time, and sample pH were optimized. High-performance liquid chromatography with UV detection was used to determine cyromazine and melamine after extraction. The proposed method was successfully applied to determination of cyromazine and melamine in egg and milk samples. Recovery of standard spiked cyromazine and melamine from these samples was between 71.86 and 80.57%, with intraday and interday relative standard deviation ranging from 3.45 to 6.39% and from 3.95 to 7.84%, respectively. The results indicate that the pseudo template M-MIP can be used for preconcentration, purification, and analysis of cyromazine and melamine in bio-matrix samples.