超高效液相色谱串联质谱法测定酒和功能饮料中3种西地那非衍生物的含量

目的建立超高效液相色谱串联质谱法(ultra performance liquid chromatography tandemmass spectrometry,UPLC-MS/MS)测定酒和功能饮料中3种西地那非衍生物(N-去甲基西地那非、吡唑N-去甲基西地那非、异丁基西地那非)含量的分析方法。方法采用Agilent Eclipse Plus C18 (3.0 mm×150 mm, 1.8μm)反相色谱柱,0.1%甲酸水和0.1%甲酸乙腈为流动相,梯度洗脱,采用多反应监测(multiplereaction monitoring,MRM)检测。结果在50～500 ng/mL的浓度范围内, N-去甲基西地那非、吡唑N-去甲基西地那非、异丁基西地那非均表现出良好的线性关系,本方法中3种化合物的检出限(limit of detection, LOD)均为15 ng/mL,定量限(limit of quantitation, LOQ)均为50 ng/mL。结论该方法操作简便,结果可靠,灵敏度高,可用于酒和功能饮料中N-去甲基西地那非、吡唑N-去甲基西地那非、异丁基西地那非含量的快速测定。     

前景看好的封闭型聚氨酯涂料

评述了近年来国外开发的以3,5－二甲基吡唑,1,2,4－三唑,或二者混用作为封闭剂的新型OEM单组分聚氨酯涂料。     

含三氟甲基芳基吡唑甲酰脲的衍生物的合成与结构表征

合成了10个新型含三氟甲基芳基吡唑甲酰脲类化合物,其结构经IR1、HNMR、元素分析确证。     

7H-pyrazolo[5, 1-a]benz[d,e]isoquinolin-7-ones: Yellow to orange dyes for synthetic-polymer fibres

N-Amino-1,8-naphthalimides were condensed with ketones containing an α-methylene group and the resulting hydrazones ring closed to afford derivatives of 7H-pyrazolo(5,1-a)benz(d,e)isoquinolin-7-one. These compounds coloured synthetic-polymer fibres, particularly polyester, in brilliant fluorescent greenish-yellow to orange hues of good fastness to light and sublimation. The colour of the dyes is discussed with respect to substituent effects in the pyrazole and naphthalene rings, and in relation to analogous 7H-benzimidazo(2,1-a)benz(d,e)isoquinolin-7-ones.     

吡唑合成的一种新方法

以甘油和水合肼为原料,在催化剂的作用下,一锅法合成吡唑,经中和、萃取、蒸馏得产品纯度≥99.5%,综合收率85.6%。     

5-氨基-1-（2-羟乙基）吡唑的合成工艺优化

5-氨基-1-（2-羟乙基）吡唑是第4代硫酸头孢噻利的C-3位侧链。用乙氧亚甲基氰乙酸乙酯和羟乙基肼为原料,经环合、水解等一锅反应合成5-氨基-1-（2-羟乙基）-4-甲酸吡唑,然后加热脱羧得到5-氨基-1-（2-羟乙基）吡唑。分析了反应原理,优化了合成条件,提高了收率,减少了副产物的产生。     

Alternatives toward proton conductive anhydrous membranes for fuel cells: Heterocyclic protogenic solvents comprising polymer electrolytes

Fuel cells are gaining increasing attention as a clean and promising technology for energy conversion. One of the key benefits of fuel cells compared to other methods is the direct energy conversion that enables the achievement of high efficiency. The electrolyte membrane is the most essential parts of a fuel cell unit, and consequently has been the subject of considerable research and development. Among the various types of proton conducting electrolytes examined for fuel cell applications, polymer electrolyte membranes (PEMs) are regarded as viable candidates since they enable operation of the cells at desirably low temperatures. This review describes recent progress in the design and development of high performance proton conducting PEMs, including the analysis of the design requirements and strategies for development of advanced PEMs for operation in anhydrous conditions. Some of the most widely used types of azole heterocycles are introduced and compared, particularly in terms of their performance characteristics in polyacids containing different functional groups. In addition, the latest research studies and progress in the field of azole-containing and azole-functionalized electrolyte systems are discussed and reviewed.     

微波辅助下4-碘吡唑衍生物的合成新方法

吡唑衍生物在碘单质和硝酸水溶液的共同作用下发生碘代反应,生成标题化合物。在微波辐射下,该方法反应速度较常规加热方法增加20倍以上,以较高产率得到了6个4-碘吡唑衍生物,收率85%～94%。     

吡唑衍生物的合成与细胞毒性研究

设计合成了七个吡唑类化合物,通过1H NMR和质谱分析对所合成的化合物进行了结构表征,并且用四甲基偶氮唑蓝(MTT)染色法测试了它们对Bel-7402(人肝癌细胞)、KB(口腔表皮样癌细胞)、HL-60(白血病细胞)和BGC-823(胃腺癌细胞)四类癌细胞株的细胞毒性,测试结果表明,4f对Bel-7402和BGC-823细胞株有较高的细胞毒性。     

吡唑席夫碱化合物的合成及其生物活性研究

以乙酰丙酮、水合肼、取代苯甲醛为起始原料,经过肟化、缩合反应得到一系列新型吡唑席夫碱化合物,通过元素分析、。HNMR、FTIR、MS等对目标化合物结构进行表征,并采用平皿法测试了目标化合物对单子叶植物玉米的生长调节活性。结果表明,目标化合物在低浓度下对玉米的生长表现出促进作用,尤以10mg·L-1浓度下对玉米生长的促进作用最显著,高浓度下对玉米的生长表现出显著抑制作用。