Use of Two-Dimensional Liquid Chromatography Combined with Diode-Array and Mass Spectrometric Detection for Analysis of Compounds in Flos Lonicera

Comprehensive two-dimensional liquid chromatographic separation by means of a combination of ion-exchange chromatography (IEC) and reversed-phase liquid chromatography (RPLC) has been realized and applied to the analysis of components of a traditional Chinese medicine Flos Lonicera. In the first dimension the components of a Flos Lonicera extract is separated on strong anion-exchange (SAX) column according to the charge-exchange properties of the components. In the second dimension the components are further fractionated by reversed-phase liquid chromatography (on ODS) on the basis of their hydrophobicity. The RPLC effluent is desalted and split and the components are identified on-line by use of both diode-array detection and mass spectrometry with atmospheric pressure chemical ionization (APCI–MS). In this way, the extract of Flos Lonicera can be rapidly separated, desalted, and analyzed, with determination of molecular weight. More than 58 components of an extract of Flos Lonicera were well resolved and six were tentatively identified from their UV and mass spectra.     

衬钽管石墨炉中小量氢气的影响及稀土基质激光晶体中铕的测定

通过纯氩中加入小量氢气,研究了保护气体对衬鉏管石墨炉分析性能的影响,结果表明,采用5％H_2-Ar作保护气体,可以显著提离衬鉏管的成品率,明显延长衬鉏管的使用寿命,使衬钽管的测定重现性得到改善,而对测定灵敏度没有明显影响。干扰试验表明,本方法可直接用于稀土基质激光晶体中铕的测定,分析结果与计算值基本一致。     

锌试剂分光光度法测定壳聚糖含量

利用锌试剂与壳聚糖在一定酸度条件下的特异性显色反应，即其复合物在465nm处吸光度与壳聚糖含量在0～O．04g／L范围内呈现良好的线性关系(R=0．996)，基于此建立了一种简便快速的分光光度法。平均回收率为99．68％。     

衬钽管石墨炉原子吸收法测定痕量镓时基体改进剂的研究及应用

提出用钒和铜混合基体改进剂衬钽管石墨炉原子吸收测定镓的方法。衬钽管使镓的灵敏度提高6倍左右,钒和铜混合基体改进剂不仅能进一步提高灵敏度,而且能提高灰化温度,降低原子化温度,增强抗干扰能力。测定 GSD 标准样品中的镓时,不需对样品进行预分离即可直接进行测定,结果与参考值相符。     

极谱杂多酸吸附波测定合金中硅

在pH2—4的盐酸介质中,硅(Ⅳ)、锑(Ⅲ)与铝(Ⅵ)形成三元杂多酸,此三元杂多酸在0.4mol/L的HCl中能迅速在滴汞电极上还原而产生灵敏的极谱电流。其峰电位为-0.30V(vs.SCE)。测定下限是8×10~(-8)mol/L。     

杯芳烃的配位化学──Ⅳ.对叔丁基杯[8]芳烃与钙、镉配合物的合成与表征

本文合成了对叔丁基杯[8]芳烃(H₈L)与钙、镉的固体配合物。并以元素分析、核磁共振、热谱、红外谱、紫外谱等进行表征。其配合物的组成分别为Ca(H₆L)·6dmf及Cd(H₆L)·6dmf.     

Hypervalent Iodine(III) Sulfonate Mediated Synthesis of Imidazo[1,2‐a]pyridines

A direct and efficient method for the conversion of alkyl aryl ketones to imidazo[1,2‐α]pyridines has been developed based on initial formation of α‐organosulfonyloxy ketones and their subsequent cyclocondensation by 2‐aminopyridines in one‐pot conditions.     

甲醇与乙醇一步合成异丁醛用CuO-ZnO/Al2O3催化剂

在ＣｕＯ－ＺｎＯ／Ａｌ２Ｏ３催化剂上，甲醇与乙醇在常压和２１０￣３６０℃温度下一步反应合成异丁醛。利用正交设计方法，研究了ＣｕＯ－ＺｎＯ／Ａｌ２Ｏ３体系催化剂组成和制备条件等因素对催化剂催化性能的影响。结果表明，催化剂中ＣｕＯ含量对催化剂的催化活性影响最大，而ＺｎＯ含量则主要影响催化剂对异丁醛的选择性。催化剂制备条件，如沉淀温度、陈化时间等，也不同程度也影响催化剂的催化性能。ＸＲＤ和ＢＥＴ表征结果     

New catalytic effect of thiourea on the oxidative cyanation of N-aryltetrahydroisoquinolines

Thiourea itself has been introduced as a mild and efficient organocatalyst for the oxidative α -cyanation of N-aryltetrahydroisoquinolines (THIQs) with trimethylsilyl cyanide (TMSCN), giving the corresponding products in good to excellent yields. Experimental investigations demonstrated that thiourea acts as a radical initiator by abstracting hydroxyl radical (OH) from tert-butyl hydroperoxide (TBHP) directly instead of non-covalent hydrogen bondings (H-bondings) activation. The use of thiourea as a radical initiator offers a new avenue for innovative chemical transformations in organocatalyzed radical chemistry.