阳离子交换色谱及动态涂层毛细管电泳法检测牛奶中乳铁蛋白含量

建立了阳离子交换色谱及动态涂层毛细管电泳检测牛奶中乳铁蛋白含量的新方法。通过purolite C115-E弱酸性离子交换树脂对牛奶中的乳铁蛋白进行提取,运用季铵化纤维素(QC)对毛细管动态涂层并测定乳铁蛋白含量。实验结果表明,该动态涂层能有效抑制毛细管内壁对乳铁蛋白的吸附。通过对QC浓度、运行缓冲液pH值、孵育时间等萃取和电泳条件的优化,实现了对牛奶样品中乳铁蛋白的定量分析。结果显示,低、中、高3个浓度组的加标回收率为87%~112%,相对标准偏差(RSDs)为4.4%~12.1%。该方法分析速度快、分离效率高、所需牛奶样品少,适用于牛奶中乳铁蛋白的分离分析。     

牛奶样品中新霉素残留量的离子色谱法测定

建立了阴离子交换色谱-脉冲安培检测分析牛奶中新霉素残留量的方法.实验采用三氯乙酸沉淀蛋白,弱阳离子交换固相萃取柱富集净化,处理牛奶样品,并考察了三氯乙酸浓度、样品过柱速度以及洗脱剂浓度等因素对牛奶中新霉素测定结果的影响.牛奶中新霉素的回收率在50.3%～76.9%范围内,基底加标工作曲线的相关系数为0.9949(n=6),线性范围为10.0～160.0ng/mL.所建立的方法可满足牛奶中低新霉素残留量的检测需要.     

基于非线性化学指纹图谱技术测定婴幼儿羊奶粉中掺假牛奶粉含量

采用非线性化学指纹图谱技术,及最小二乘一元线性回归方法对婴幼儿羊奶粉中掺假牛奶粉进行定量分析。首先测定具有不同掺杂百分比的混合奶粉标样非线性化学指纹图谱,利用其停波时间相对于掺杂牛奶粉含量之间的一元线性关系,通过最小二乘法建立测定混合奶粉中掺杂牛奶粉含量的校正模型;然后用该模型和混合奶粉试样指纹图谱的停波时间来计算混合奶粉中掺杂牛奶粉的含量;最后根据掺杂牛奶粉的含量来鉴别和定量评价奶粉质量。实验表明:该方法相关系数为0.9945,相对标准偏差(RSD)为0.53%~2.18%,回收率在95.3%~107.0%范围,检出限为1.09%。方法准确度高,重现性好,操作简单,是一种切实可行的测定婴幼儿羊奶粉中掺杂牛奶粉含量的方法。     

环境友好型方法快速检测牛奶中的六种喹诺酮残留

本文建立了一种环境友好型、同时分离检测牛奶中六种喹诺酮类药物的高效液相色谱分析法。方法采用反相Chromatorex C18色谱柱,二极管阵列检测器,检测波长为280 nm。实验表明,适当浓度的柠檬酸和硫酸铵溶液作为提取液时可使牛奶中的蛋白质发生缓慢而彻底的变性,释放出与其结合的喹诺酮类药物,从而提高了从牛奶中提取喹诺酮类药物的提取效率。然后通过对提取液进行加热沉淀蛋白质、加入PSA(N-丙基乙二胺修饰的硅胶)净化,即可实现样品的快速前处理。该方法用于牛奶中六种喹诺酮类抗生素残留的测定,回收率均在82.0%～117.8%之间,方法检出限为34.5～85.0 ng·g-1。本文提出的样品前处理方法可靠、快速、环保、易于操作。     

单分散Au纳米粒子液相合成与快速检测三聚氰胺——本科生综合化学实验

利用Au纳米粒子与三聚氰胺相互作用产生的颜色变化来快速评估牛奶中三聚氰胺的含量,采用透射电子显微镜表征Au纳米粒子与三聚氰胺作用前后的形貌变化,通过用紫外-可见吸收光谱数据绘制标准工作曲线来定量测定牛奶中三聚氰胺的含量。该实验贴近生活,学以致用,同时也有助于学生掌握无机化学和分析化学基本操作,对增强学生分析解决问题的能力,提升学生的科研素养也有帮助。     

牛奶中酪蛋白和乳糖的分离及纯度测定

分离牛奶中的酪蛋白和乳糖,并对其纯度进行测定。以此作为物理化学设计实验的部分内容。     

牛奶的保鲜

本文介绍了牛奶的保鲜方法,说明了牛奶致腐的原因,概述了因微生物的作用所导致的牛奶中乳糖、蛋白质和脂肪3种主要成分的变化,并简单介绍了这些变化的反应机理。     

分子印迹固相微萃取-高效液相色谱法测定水和牛奶中三种四环素类药物

以土霉素为模板分子制备了分子印迹固相微萃取涂层,建立了选择性萃取、高效液相色谱法同时测定牛奶和水样中四环素、盐酸土霉素和金霉素三种四环素类抗生素的分析方法。将0.1mmol盐酸土霉素在功能单体和交联剂的作用下制备分子印迹预聚合液,将经多巴胺处理后的不锈钢丝前端1~2cm置入其中,制备分子印迹固相微萃取涂层。3mL牛奶和水样经涂层萃取50min、解析5min,乙腈-10mmol/L磷酸盐缓冲液(PBS,pH=3)作为流动相,二极管阵列检测器(DAD)定量分析。实验结果表明,分子印迹涂层对四环素类目标物的特异性选择明显优于非印迹涂层。三种目标抗生素在100~1 000μg/L(牛奶)和10~1 000μg/L(水样)浓度范围内线性关系良好,相关系数在0.9959以上,四环素、盐酸土霉素和金霉素的检出限(S/N=3)为40~80μg/L(牛奶)和5~10μg/L(水样);加标水平为500μg/L时,回收率范围97.8%~109.0%,相对标准偏差(n=7)分别为5.3%~8.2%(牛奶),3.7%~6.4%(水样)。该方法前处理简单、绿色环保、选择性好、精密度好、回收率高,可用于牛奶和水样中上述三种四环素的实际检测。     

金纳米粒子比色探针检测牛奶及鸡蛋中的三聚氰胺

三聚氰胺能诱导金纳米粒子(AuNPs)团聚,溶液颜色由酒红色变为紫色或蓝灰色.以AuNPs作为比色探针,建立了快速检测牛奶和鸡蛋中三聚氰胺的方法.实验优化得最佳反应条件为:AuNPs粒径13 min、pH=7、反应时间10 min和温度为室温.对样品中常见物质进行了干扰实验.样品经10％三氯乙酸和氯仿提取、离心分离后可...     

基于二维相关近红外光谱判定牛奶中掺杂的目标物

分别配制含有不同浓度尿素(1～20g.L-1)、葡萄糖(1～20g.L-1)和三聚氰胺(0.01～3g.L-1)的牛奶溶液共120个,采用二维相关近红外光谱对掺杂牛奶进行了快速判别分析。以牛奶中掺杂目标物浓度为外扰,构建二维相关近红外光谱,研究了各掺杂牛奶的二维相关近红外特性,并进行对比、分析。掺杂尿素牛奶在同步图上出现两个较强的自相关峰,分别在4 552,4 648cm-1处;掺杂葡萄糖牛奶,在同步图中出现3个较强的自相关峰,分别在4 456,4 392,4 360cm-1处;而掺杂三聚氰胺牛奶也有两个较强的自相关峰,出现在4 256,4 328cm-1处。结果表明:所提出的方法能实现对含有上述掺杂物牛奶的正确识别,为快速判别牛奶的安全性提供新方法。     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

正丁胺对激光染料荧光谱影响的研究

用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu⁰ as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than Cu^I in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C₆₀, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine.