Structure-driven design and synthesis of chiral dioxocyclam derivatives

Based on an analysis of previously reported structures and a potential geometry fit with substrates, a new family of chiral dioxocyclam derivatives have been designed. The synthesis of those ligands was accomplished starting from l-proline and α-d-amino acids (converted to β-amino acids) with a key step of macrocyclization reaction of amino esters. All ligands were converted into neutral copper(II) complexes (amide groups underwent deprotonation of upon treatment of ligands with copper(II) acetate). The complexes exhibit the desired shape of their active surfaces, as proved by X-ray analysis.     

工业氨基三甲叉膦酸中副产物的核磁共振分析

采用多种核磁共振(NMR)技术测定了工业氨基三甲叉膦酸(ATMP)产品中副产物的分子结构，发现该物质为甲氨基二甲叉膦酸(MADMP)，它是甲醛歧化反应导致的副产物；给出了可能的反应方程式；测出了MADMP的相对含量，MADMP与ATMP摩尔比约为2。     

A specific colorimetric cysteine sensing probe based on dipyrromethane-TCNQ assembly

A new charge-transfer complex, consisting of dihydroxymethyl di-(2-pyrrolyl)methane and tetracyanoquinodimethane (TCNQ), has been designed to high selectively distinguish cysteine from other amino acids in water/organic solvent mixtures through the visual color change from blue to nearly colorless. The excellent system properties make the supramolecular assembly a highly selective colorimetric probe for monitoring cysteine.     

L-赖氨酸锌兔体内生物利用度研究

用原子吸收分光光度法和氨基酸自动分析仪法分别测定兔血清锌浓度和血清L-赖氨酸含量．结果表明．L-赖氨酸锌中锌的相对生物利用度明显优于硫酸锌．而其中的L-赖氨酸的相对生物利用度与L-赖氨酸组比较无明显差异．     

高效液相色谱法检测保健食品中大豆异黄酮含量

建立了保健食品中大豆异黄酮的高效液相色谱检测方法 ,通过正交试验法得出保健食品中大豆异黄酮的最佳水解条件为 :盐酸浓度2.0mol/L,酸体积40mL ,水解温度80℃ ,水解时间3h;采用HypersilODS2C18 色谱柱 (250mm×4.6mmID ,5μm) ,流动相为甲醇 -水(体积比47∶53) ,流速1.0mL/min ,检测波长260nm ,柱温40℃ ,线性范围在0.5～96mg/L ,相关系数r为0.999 ,相对标准偏差 (RSD)2.09% ,回收率在98.5 %～100.5 %。     

α-氨基酸-丁醇-水三元体系中分子间的异系焓相互作用

利用2277热活性检测仪的流动测量系统获得了298.15K时甘氨酸、L-丙氨酸、L-缬氨酸和L-脯氨酸分别与n-丁醇在水溶液中混合过程的焓变以及各自的稀释焓,依据McMillan-Mayer理论关联得到异系焓相互作用系数,讨论了不同氨基酸与n-丁醇分子的作用机理.对hxy值分析结果表明,不同氨基酸与n-丁醇分子间的异系焓作用系数的大小主要取决于氨基酸分子结构的差异,氨基酸的不同侧基(非极性或极性)对焓作用系数有着不同的贡献,焓作用系数值的相对大小最终取决于各基团之间竞争平衡的结果.脯氨酸特殊的五元吡咯环结构对hxy值有较大的正贡献;n-丁醇的疏水性比尿素或甲脲大得多.     

Separation of enantiomers in capillary electrophoresis with contactless conductivity detection

Contactless conductivity detection is successfully demonstrated for the enantiomeric separation of basic drugs and amino acids in capillary electrophoresis (CE). Derivatization of the compounds or the addition of a visualization agent as for indirect optical detection schemes were not needed. Non-charged chiral selectors were employed, hydroxypropylated cyclodextrin (CD) for the more lipophilic basic drugs and 18-crown-6-tetracarboxylic acid (18C6H4) for the amino acids. Acidic buffer solutions based on lactic or citric acid were used. The detection limits were determined as 0.3 microM for pseudoephedrine as an example of a basic drug and were in the range from 2.5 to 20 microM for the amino acids.     

Decolorization of AZO dyes using catalytic ozonation

Decolorization of C.I. Reactive Red 2 (RR2) and C.I. Acid Orange 6 (AO6) using a catalytic ozonation system was evaluated. The decolorization rates for RR2 and AO6 were accelerated by at least 30% by adding MnO₂ to the O₃ system; additionally, the decolorization rate increased as the MnO₂ dosage and ozone power consumption increased. Enhanced MnO₂ catalytic ozonation was more apparent for AO6 than for RR2.     

Simple and rapid quantitative determination of lysinoalanine and protein hydrolysate amino acids by high-performance liquid chromatography after derivatization with dansyl chloride

Summary A rapid and simple method for the determination of both lysinoalanine (LAL) and protein hydrolysate amino acids after derivatization with dansyl chloride (5-dimethylaminoaphtalene-1sulfonyl chloride) and separation with RP-HPLC (UV detection) is presented. LAL is analysed in less than 15 minutes and complete separation of 22 amino acids is achieved in less than 30 minutes using single linear gradients of solvents (phosphate buffer and acetonitrile). Quantitative results obtained by HPLC compare well with results of the ion-exchange chromatography (amino acid analyser). The importance of the duration of the derivatization reaction and of the excess of reagent is discussed. As examples, the results of the determination of LAL in two samples of base treated α-casein and 22 samples of soy protein and the results of the analysis of amino acids in two balanced diet mixtures are presented. Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984