十六烷基三甲基溴化铵光度滴定法测定硫酸外国佬骨素钠盐

建立一种测定硫酸软骨素的新方法。十六烷基三甲基溴化铵在KH2PO4-Na2HPO4缓冲溶液中、乳化剂OP共存下与硫酸软骨素反应形成离子对缔合物，溶液转变成稳定的乳化液。用光度滴定法测定硫酸软骨素。用标准加入法做加收试验，回收率为99.9%-100.2%，相对标准偏差0.32%-0.40%。方法应用于外贸样品测定，结果满意，方法准确、简便、快速。     

鱼翅中硫酸软骨素的酶解-高效液相色谱法测定

建立了一种测定鱼翅中硫酸软骨素的酶解－高效液相色谱方法；该法利用在一定条件下硫酸软骨素能被硫酸软骨素酶ABC定量酶解成软骨素二糖，通过高效液相色谱法测定软骨素二糖的量来计算硫酸软骨素的含量。     

酸水解-柱前衍生化-HPLC-MS/MS法分析三种即食海产品中的酸性多糖

从扇贝丁、鱿鱼丝和鳕鱼片中提取得到粗多糖,使用1.3 mol/L的三氟乙酸(TFA)进行降解,1-苯基-3-甲基-5-吡唑啉酮(PMP)柱前衍生化后,高效液相色谱-三重四级杆质谱(HPLC-MS/MS)分析降解产物中的二糖片段。扇贝丁和鱿鱼丝中的酸性多糖几乎全部为硫酸软骨素;而鳕鱼片不仅含有硫酸软骨素,还含有少量透明质酸,相对含量分别为87.5%和12.5%。     

基于离子液体的反相液相色谱法检测胆碱和四甲基铵

本文发展了以离子液体为流动相添加剂的反相液相色谱分离和间接紫外检测胆碱和四甲基铵的方法。研究了离子液体、甲醇、紫外检测波长等因素对分离、检测胆碱和四甲基铵的影响。用普通的反相色谱柱，以甲醇/1-丁基-3-甲基咪唑四氟硼酸盐水溶液为流动相，在210 nm紫外检测波长下，实现了胆碱和四甲基铵的分离和检测。本方法对分析物的检出限低于0.5 mg/L,标准曲线具有良好的线性关系。将方法应用于植物生长调节剂和桶装水样品的分析，加标回收率为95.1%～99.6%,相对标准偏差小于2.0%。     

问题肝素中多硫酸软骨素杂质的柱前衍生高效液相色谱分析

基于肝素和多硫酸软骨素(OSCS)在单糖组成上的差别,建立了可用于肝素中OSCS检测的柱前衍生高效液相色谱法.采用3 mol/L三氟乙酸,将受污染的问题肝素在110℃下充氮封管水解4 h,在碱性条件下与1-苯基-3-甲基-5-吡唑啉酮进行衍生化反应,再采用C18反相色谱柱,以0.1 mol/L磷酸盐(pH=6.7)缓冲液/乙腈(体积比82∶18)为流动相,在流速1.0 mL/min、柱温25℃及紫外检测波长245 nm的条件下进行液相色谱分析.结果表明,肝素和OSCS的单糖色谱峰具有良好的分离度,测得2批问题肝素中OSCS杂质的质量分数分别为19.6%和28.3%.该方法具有良好的精密度和重现性,易于推广,适合于肝素中OSCS杂质的检测,并可用于硫酸软骨素A和C与硫酸软骨素B的区分和鉴别.     

以离子液体为流动相的高效液相色谱-间接紫外检测法分析四甲基按根离子

建立了四甲基铵根离子的反相高效液相色谱-间接紫外检测分析法.以ZORBAX ODS反相色谱柱为分离柱,采用间接紫外检测方法,考察了紫外检测波长和离子液体+有机溶剂(乙腈、甲醇)流动相对分离和测定四甲基铵根离子的影响.最佳色谱条件为:以80% 1-乙基-3-甲基咪唑四氟硼酸盐水溶液(0.5 mmol/L,乙酸调pH 3....     

甲基紫硫酸软骨素共振瑞利散射光谱及其应用

在Britton-Robinson缓冲介质(pH9.37)中硫酸软骨素与甲基紫反应形成离子缔合物时,共振瑞利散射(RRS)强度会明显增强,其最大RRS峰位于505和661 nm处。本文对反应的最佳条件、影响因素、硫酸软骨素浓度与RRS强度的关系进行了研究,建立起一种快速、简便、灵敏的测定硫酸软骨素的方法。本法在661和505 nm测定波长处的线性范围均为:0.15~0.90 mg/L,其检出限分别为0.019 mg/L(505 nm)和0.043mg/L(661 nm)。该法应用于针剂中硫酸软骨素的测定,结果满意。     

用电活性离子对制成的离子选择电极测定阳离子表面活性剂

制备了3种基于不同电活性物质(十二烷基二甲基苄基铵-四苯硼、十六烷基三甲基铵-四苯硼、十八烷基三甲基铵-四苯硼)的阳离子表面活性剂离子选择电极,并对其性能做了测定,结果显示该类电极对阳离子表面活性剂十二烷基二甲基苄基氯化铵、十六烷基三甲基溴化铵、十八烷基三甲基氯化铵均有能斯特响应。以此类电极作为指示电极,四苯硼钠溶液作为滴定剂,对阳离子表面活性剂(十二烷基二甲基苄基氯化铵、十八烷基三甲基氯化铵、海明1622)进行了活性物含量的测定,与两相滴定法测定结果进行了比较。     

十六烷基三甲基溴化铵光度滴定法测定硫酸软骨素钠盐

建立一种测定硫酸软骨素的新方法。十六烷基三甲基溴化铵在KH2 PO4 Na2 HPO4 缓冲溶液中、乳化剂OP共存下与硫酸软骨素反应形成离子对缔合物 ,溶液转变成稳定的乳化液。用光度滴定法测定硫酸软骨素。用标准加入法做回收试验 ,回收率为 99.9%～ 10 0 .2 % ,相对标准偏差0 .32 %～ 0 .4 0 %。方法应用于外贸样品测定 ,结果满意 ,方法准确、简便、快速     

中性红光度法测定硫酸软骨素含量

硫酸软骨素是一种天然酸性粘多糖，属生物高分子化合物。硫酸软骨素有A、C和D三种异构体，均是由D-葡萄糖醛酸和N-乙酰-D氨基半乳糖组成，只是硫酸基位置不同。硫酸软骨素具有许多重要的生理活性和药理作用，如促进冠状动脉循环、降血脂、抗凝血、抗肿瘤和防止血管硬化等，广泛用于临床、化妆品和医用材料等领域。硫酸软骨素的测定方法有Elson-Morgan反应法，即将硫酸软骨素水解或酶解成氨基己糖，然后在碱性条件下与乙酰丙酮反应，生成色原，再与对二甲氨基苯甲醛的盐酸醇溶液反应产生红色，以盐酸氨基葡萄糖为对照品，用比色法测定。还有高效液相色谱法，天青A和亚甲基蓝吸收光谱法。中性红属于醌亚胺类染料，带正电荷，曾作为生物标记用于做蛋白质和DNA的光谱探针。本文将中性红作为糖类物质的光谱探针，研究了中性红与硫酸软骨素的相互作用，根据其复合物溶液在特定波长处吸光度降低与硫酸软骨素的含量成比例的特点，建立了一种快速、简便、灵敏的测定硫酸软骨素含量的光度法。     

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.     

A carbanion induced synthesis of highly congested pyrazole and imidazole containing heterocycles

An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.     

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.     

Selective synthesis of 4,5-dihydroimidazo- and imidazo[1,5-a]quinoxalines via modified Pictet–Spengler reaction

An efficient tandem approach for the selective synthesis of 4,5-dihydroimidazo[1,5-a]quinoxalines 6a–g and imidazo[1,5-a]quinoxalines 7a–h by the reaction of 2-imidazolyl anilines 4a–c with aryl aldehydes 5a–k under mild reaction conditions is described. Introduction of electron releasing alkyl groups in substrates 4a–b was found to be instrumental for the success of the reaction.     

Understanding the Diels-Alder reactivity of 1,2-azaborine analogues

The Diels-Alder reactivity of 1,2-heteroborines (H₄C₄B(H)X, X?=?NH, PH, AsH; O, S, Se) has been computationally explored by means of Density Functional Theory (DFT) calculations. The influence of the HB?=?X fragment on the reactivity of the system has been quantitatively analyzed in detail by means of the so-called Activation Strain Model (ASM) of reactivity. It is found that the interaction between these species and the dienophile is significantly stronger than that computed for their all-carbon isoelectronic counterpart, benzene. In addition, the strain energy plays a key role in the observed reactivity trends. The role of the aromaticity strength of these heteroarenes on the reactivity is also assessed.