Determination of Melamine in Dairy Products and Melamine Tableware by Inhibition Electrochemiluminescent Method

An electrochemiluminescent (ECL) method has been developed for the determination of melamine based on the inhibition of luminol ECL. A significant luminol ECL can be found at 1.47 V in the phosphate buffer solution at high pHs and low potential scan rates, this ECL signal can be inhibited obviously by melamine. The decrease of ECL intensity was linearly proportional to the logarithm of melamine concentration in the range of 1–100 ng/mL (R²=0.9911) and with the detection limit of 0.1 ng/mL. The method has been applied successfully to determine melamine in dairy products and melamine tableware, the recoveries were in the range of 98.5%–103.7% and 95.5%–106.0%, respectively. The mechanism of the inhibition effect was also proposed, the active oxygen (O₂^{· −}) generated from the electrooxidation of OH⁻ reacted with luminol anion (L^{· −}) to generate light emission, and the present of melamine can eliminate the active oxygen, which cause the decrease of the ECL intensity.     

超高效液相色谱-串联质谱法同时测定牛奶和奶粉中的二氰二胺、三聚氰胺和三聚氰酸

建立了一种超高效液相色谱-串联质谱法测定牛奶和奶粉中二氰二胺(DCD)、三聚氰胺(MEL)和三聚氰酸(CY)的分析方法。样品用5%(质量分数)三氯乙酸水溶液提取,无需净化和浓缩,用Acquity UPLC HSS T3色谱柱(50 mm×2.1 mm, 1.8 μm)分离,以乙腈和乙酸铵作为流动相进行梯度洗脱,电喷雾正、负离子(ESI^±)模式同时电离,多反应监测模式进行检测。结果表明:在5.0～200.0 μg/L范围内线性关系良好(r≥0.995)。牛奶中3种化合物在0.02、0.10、0.20 mg/kg的添加回收率为60.0%～105.8%,相对标准偏差(RSD, n=6)为4.2%～13.6%;奶粉中3种化合物在0.05、0.10、0.20 mg/kg的添加回收率为78.0%～115.0%, RSD (n=6)为2.7%～7.5%。牛奶中方法的定量限(信噪比为10)为0.02 mg/kg,奶粉中方法的定量限为0.05 mg/kg。该方法简单、快速、灵敏、准确,适合于牛奶、奶粉等乳及乳制品中DCD、MEL和CY的快速、高灵敏的分析检测。     

Melamine Trisulfonic Acid (MTSA): A New Efficient Catalyst for the Chemoselective Methoxymethylation of Alcohols

Melamine trisulfonic acid, which is easily prepared by the reaction of melamine with neat chlorosulfonic acid, is able to efficiently catalyze the chemoselective methoxymethylation of alcohols with dimethoxymethane (DMM). All reactions were performed under mild and completely heterogeneous reaction conditions in good to high yields.     

碳载高分散钯纳米粒子的制备及催化Suzuki反应

利用三聚氰胺甲醛预聚物中N原子与Pd²⁺的相互作用,将Pd²⁺化学锚定在预聚物中;并以二氧化硅水凝胶为造孔剂、2,4-二氨基苯磺酸为预聚物缩合促进剂,在水溶液中制备出锚定了Pd²⁺的胶体纳米球;再经摩尔分数5%氢气焙烧、HF腐蚀,得到Pd质量分数为1.37%、平均粒径为(2.4±0.87) nm的碳载高分散Pd纳米粒子催化剂Pd@C。 将其应用于Suzuki反应,在加入Pd与碘苯物质的量比为1:100的催化剂时,反应5 min收率为99.3%,且经8次循环后活性未降低,表现出良好的催化效果和重复使用性。     

汽车罩光清漆的固化和降解机理研究(Ⅱ)--用色谱质谱,核磁共振和红外光谱等方法研究罩光清漆的主要成分和结构

罩光清漆的色谱质谱(GC/MS),13C,1H液体高分辨核磁共振(NMR)和红外光谱(IR)等多种方法的综合分析结果表明,新型汽车涂料主要是由丙烯酸丁酯,丙烯酸1,2-丙二醇酯等形成的丙烯酸酯共聚物和部分丁氧基化的三聚氰胺甲醛树酯交联剂所组成,它们溶解在由多种有机溶剂组成的混合溶剂中.     

氮掺杂石墨烯的制备及其氧还原电催化性能

以三聚氰胺和氧化石墨烯(GO)为原料,经物理研磨和高温热解得到氮掺杂石墨烯(三聚氰胺-NG).扫描电子显微镜(SEM)测量显示,所制备的三聚氰胺-NG厚度和表面褶皱较掺杂前略有增加.X射线光电子能谱(XPS)表明,在三聚氰胺-NG中氮元素以吡咯N、吡啶N和石墨N 3种形式掺杂在石墨烯中,它们的比例分别是14.5%、24.5%和61.0%.同时运用循环伏安法(CV)和旋转圆盘电极技术(RDE)测试了三聚氰胺-NG在碱性介质中的氧还原电催化活性.结果表明,与商业石墨烯和由聚吡咯为氮源制备的氮掺杂石墨烯(ppy-NG)相比,三聚氰胺-NG具有较高的电催化活性和较正的氧还原起始电位(-0.09V),并且电催化还原氧气时主要为4电子反应.由于其较高的氧还原性能和较低的成本,三聚氰胺-NG在碱性燃料电池阴极电催化剂中有良好的应用前景.     

Polyelectrolyte Multilayer Microspheres as Carriers for Bienzyme System: Preparation and Characterization

Summary: Polyelectrolyte multilayer microspheres were prepared by alternating adsorption of dextran sulfate and protamine on melamine formaldehyde cores followed by the partial decomposition of the core. Peroxidase and glucose oxidase were immobilized in the prepared microspheres. Retention of enzymatic activity of the peroxidase/glucose oxidase system incorporated into the microspheres was demonstrated. Applicability of the bienzyme system immobilized in the microspheres for kinetic glucose assay was shown.

SEM image of the polyelectrolyte multilayer microsphere.     

食品及饲料中三聚氰胺残留量液相色谱检测方法的研究

建立了食品及饲料中三聚氰胺残留检测的反相高效液相色谱方法。样品经乙腈水或甲醇水提取,离心分离,过0.2m滤膜,然后采用RP-HPLC-UV法测定,外标法定量。对色谱分离条件进行了优化,三聚氰胺在0.05g/mL～10.0g/mL范围内线性良好,相关系数为0.99994。在4.0mg/kg～80.0mg/kg浓度范围内,平均加标回收率在90.5%～102.7%之间,相对标准偏差为2.96%～3.62%,方法的最低检出限为5mg/kg。该方法简便、快速,满足食品及饲料中三聚氰胺残留量的检验工作需要。     

三聚氰胺热解产物的特性分析

以有机物三聚氰胺为初始原料, 在真空条件下使其热解（1 000 K）. 采用X射线衍射（XRD）、 透射电子显微镜（TEM）、 X射线光电子能谱(XPS)、 化学元素分析（EA）和傅里叶红外光谱(FT-IR) 分析样品的形貌、 成分和结构. 结果表明, 在真空条件下, 三聚氰胺全部分解, 分解产物为片层石墨相C₃N₄.      

锰氧化物/碳氮三维网络结构复合材料的制备及锂电性能

通过硝酸锰和乙醇的水热反应在三聚氰胺泡棉(MF)上生成三氧化二锰颗粒,氮气下高温处理后形成锰氧化物负载碳氮三维网络结构的复合物。碳氮网络结构提高了充放电过程中材料结构的稳定性及导电性,且烧结过程中产生的孔道结构有利于锂离子传输,使得该复合材料作为负极在锂离子电池中表现出优异的充放电性能和循环稳定性。材料的比容量和循环稳定性大大提高,经500℃处理后的MnO/CNnws-500材料在160次循环后仍然保留590 m Ah·g~(-1)的比容量,达到氧化亚锰理论容量755 m Ah·g~(-1)的78%。