浓缩刺梨汁中噻菌灵和多菌灵残留量的高效液相色谱法测定

研究了一种可同时测定浓缩刺梨汁中噻菌灵和多菌灵残留量的固相萃取-高效液相色谱法。浓缩刺梨汁样品与水按一定比例稀释后，经过调pH、离心、过滤，用混合相固相萃取小柱（Mixed—mode SPE）进行提取、净化，用配有二级管阵列检测器（DAD）的液相色谱仪检测，外标法定量。用噻菌灵和多菌灵对照品进行添加回收率测定，结果显示本方法对噻菌灵的测定低限为0．020mg／kg，回收率为77．5％～87．1％；对多菌灵的测定低限为0．020mg／kg，回收率为74．0％～96．3％；测定的相对标准偏差均不大于7．4％。本方法能满足常规噻菌灵和多菌灵残留量检测的需要。     

固相萃取富集高效液相色谱法测定苯氧乙酸和2，4—二氢苯氧乙酸

建立了以固相萃取技术进行富集,高效液相色谱法进行分离和检测苯氧乙酸和2,4－二氯苯氧乙酸的方法。环境水中的苯氧乙酸和2,4－二氯苯氧乙酸用Sep-Pak C18 Cartridge进行固相萃取。液相色谱的条件是：Shim-Pack CLC ODS柱为分析柱;甲醇－水（9：1,V／V）为流动相;流速为1mL/min;在UV－275nm波长下进行检测。本法具有良好的灵敏度和重现性。     

固相萃取富集-高效液相色谱法分离检测水中3种苯脲除草剂

建立了固相萃取富集-高效液相色谱分析水中3种痕量苯脲除草剂——利谷隆、敌草隆、灭草隆的方法。C18固相萃取柱富集水中待测组分,高效液相色谱以Hypersil ODS柱为分析柱,优化出的色谱条件为：流动相为甲醇／水=60：40(V／V);流速为0．7mL／min;柱温为30℃。本法操作简便、灵敏、回收率高。     

多功能柱净化-高效液相色谱法检测谷物中的玉米赤霉烯酮

建立了玉米和小麦中玉米赤霉烯酮（ZEN）的多功能柱净化-高效液相色谱检测方法。样品经乙腈-水混合溶剂（V（乙腈）：V（水）=84：16）提取，通过多功能净化柱（MFC）进行一次性净化，以Symmetry^R C18柱为分离柱，甲醇-水（V（甲醇）：V（水）=68：32）为流动相进行高效液相色谱分离和检测。玉米赤霉烯酮的质量浓度在0．01～4．0μg／mL范围内呈良好线性，相关系数为0．9996。检出限为0．04μg／g，在0、04—5．0mg／kg添加范围内的回收率为87．5％～98．6％，相对标准偏差为1．5％～8．3％。     

固相萃取富集高效液相色谱法测定苯氧乙酸和2,4-二氯苯氧乙酸

建立了以固相萃取技术进行富集 ,高效液相色谱法进行分离和检测苯氧乙酸和 2 ,4 二氯苯氧乙酸的方法。环境水中的苯氧乙酸和 2 ,4 二氯苯氧乙酸用Sep PakC18Cartridge进行固相萃取。液相色谱的条件是 :Shim PackCLCODS柱为分析柱 ;甲醇 水 (9∶1,V/V)为流动相 ;流速为 1mL/min ;在UV 2 75nm波长下进行检测。本法具有良好的灵敏度和重现性     

一种测定MDR肿瘤细胞内外阿霉素浓度的方法

研究提出K562／A细胞内外阿霉素浓度的反相高效液相色谱-荧光测定法．细胞内阿霉素浓度测定采用Lichrospher C18色谱柱，甲醇-0．01％醋酸(50：50，V／V)流动相,流速1．0mL／min，柱温35℃；细胞外阿霉素浓度测定采用Lichrospher C18色谱柱，甲醇-0．01％醋酸(55：45，V/V)流动相，流速0．8mL／min，柱温35℃．荧光检测器波长λex=495nm，λem=560nm，均以盐酸柔红霉素为内标．研究结果表明，该方法简单、准确、线性范围宽、检测限低，精确度和回收率良好，可用于多药耐药肿瘤细胞内外阿霉素浓度的动态变化规律研究．     

固相萃取富集-高效液相色谱分离和测定邻甲苯胺和邻硝基甲苯

建立了以固相萃取技术进行富集 ,高效液相色谱进行分离和检测邻甲苯胺和邻硝基甲苯的方法。污染水中的邻甲苯胺和邻硝基甲苯采用Sep pakC1 8萃取柱进行固相萃取。色谱分离条件是 :Shim PackCLCODS(1 5 0mm× 4 .6mmid ,5 μm)柱为分析柱 ,甲醇 水 =60∶4 0 (V V)为流动相 ,流速为 1 .0mL min,邻甲苯胺和邻硝基甲苯的紫外检测波长分别为 2 3 0nm和 2 5 4nm ,本法具有良好的灵敏度和重现性。     

固相萃取高效液相色谱法测定蜂王浆啤酒中的1O-羟基-2-癸烯酸

建立了固相萃取高效液相色谱法测定蜂王浆啤酒中10-羟基-2-癸烯酸含量的方法。采用固相萃取技术富集蜂王浆中的10-羟基-2-癸烯酸,以甲醇-水-磷酸(体积比为50：50：0．5)为流动相,ODS柱分离,用紫外检测器于215nm处检测。10-羟基-2-癸烯酸的浓度在0．5-100．0μg/mL范围内与其色谱峰峰面积呈良好线性关系(r=0．9999),回收率为98％-108％,RSD为2.1％。     

超高效液相色谱法测定护手霜中5种不同的雌激素

建立了超声波萃取．超高效液相色谱快速测定护手霜中5种雌激素（雌酮,雌二醇,苯甲酸雌二醇,美雌醇,炔雌醇环戊醚）的分析方法,研究了萃取溶剂、萃取时间对萃取效率的影响,确立了流动相流速及色谱柱柱温等检测条件．化妆品以乙腈和水（20：80,V：V）为提取溶剂进行超声波萃取后用C18色谱柱分离,乙腈和水溶液为流动相,梯度洗脱,10min内完成5种雌激素的分离与检测．方法的检出限为0．016—0．031μg／mL,相对标准偏差均小于5．0％m=3）,5种雌激素的工作曲线的相关系数均高于0．992．化妆品的加标回收率在85％～95％之间．方法简单快速、灵敏度高、分离效果好,满足化妆品中雌激素分析的需要．     

高效液相色谱法分离与测定柴胡中的柴胡皂甙a

采用反相高效液相色谱法对北柴胡中的柴胡皂甙a进行了分离和测定。试验选出分离的最佳条件：流动相为V（乙腈）：V（水）=90：10，流速为0．8mL／min，检测波长为208nm，在0．05—1．50mg／mL范围内柴胡皂甙a的量与峰面积线性关系良好，回归方程为：Y=2258428p＋186676，相关系数r=0．9993，检出限为2．3ng／mL，回收率为98．3％-100．9％。     

多环芳二酐型聚酯亚胺膜的透气性能

多环芳二酐型聚酯亚胺膜的透气性能李悦生，丁孟贤，徐纪平（浙江大学高分子科学与工程研究所，杭州，３１００２７）（中国科学院长春应用化学研究所）关键词聚醚酰亚胺，聚酯酰亚胺，膜，透气性通常的聚酰亚胺加工性能较差，在芳环二酐的苯环间引入醚键等柔性基团后，其...     

Determination and study on residue and dissipation of benazolin-ethyl and quizalofop-p-ethyl in rape and soil

A QuEChERS (quick, easy, cheap, effective, rugged, and safe) method for the determination of benazolin-ethyl and quizalofop-p-ethyl in rape and soil by high-performance liquid chromatography-tandem mass spectrometry has been developed in this study. The residue and dissipation of benazolin-ethyl and quizalofop-p-ethyl in rape and soil were determined with the developed method. The half-lives of benazolin-ethyl in rape straw and soil were 3.7–5.1 days and 14.3–26.3 days, respectively. The half-lives of quizalofop-p-ethyl in rape straw and soil were 5.0-6.1 days and 0.3–9.7 days, respectively. The residue of benazolin-ethyl and quizalofop-p-ethyl in rapeseed and soil were below the detection limit (i.e., 0.5?mg?kg^?1, the maximum residue level of European Union for quizalofop-p-ethyl).     

微量元素与疾病诊断治疗的研究现状及展望

对国内外微量元素与疾病的关系及其诊断治疗的研究现状及研究动向进行了综述，包括：微量元素与地方病、癌肿、心血管病、糖尿病、眼病、神经系统病等。参考文献72篇。     

Ferrocene and ferrocenium modified clays and their styrene and EVA composites

In this work, ferrocene- and ferrocenium-containing salts were employed to modify montmorillonite. X-ray measurements show an increase in the interlayer spacing upon clay modification, which means that the larger and more organophilic cations were inserted into the gallery space of montmorillonite. Attempts to prepare nanocomposites of polystyrene and ethylene vinyl acetate copolymers lead to immiscible systems; the morphology of these systems was elucidated with TEM, XRD and cone calorimetry. The thermal stability of the composites is greater than that of the virgin polymer.     

Ti-V基储氢合金及其氢化物的物相结构与组分优化设计

Ti-V基储氢合金在室温、常压下即可表现出良好的储氢特性,且质量储氢容量明显高于传统AB₅型储氢合金,从而在氢气的精制和回收、运输和储存及热泵等方面有较早的应用。 此外,在混合气体分离、核反应堆中处理氢的同位素、镍氢电池及燃料电池负极材料等方面也得到了广泛的研究与关注。 基于目前Ti-V基储氢合金的研究现状,概述了该类合金的优势、限制性因素(包括成因)及改性手段。 此外,为了进一步理解Ti-V基合金储氢机理、构建合金组分与储氢特性之间的对应关系,本工作重点围绕Ti-V基储氢合金及其氢化物的结构、组分优化设计展开综述,并对其未来研究方向做出展望。     

钒与糖代谢及糖尿病

微量元素钒作为生物体内必需元素，经证实有很重要的生理学功能，与机体糖代谢有十分密切的关系，且能降低糖尿病动物模型的高血糖，极有可能被开发为治疗糖尿病的药物。     

Synthesis and Optical and Redox Properties of Symmetric and Asymmetric BODIPYs

Herein, we present the synthetic route and the photophysical, electrochemical as well as laser properties of novel red‐emitting boron‐dipyrromethenes (BODIPYs) bearing arylethyne moieties. Such functionality is added along the main axis of the chromophore leading to single‐ and double‐substituted derivatives. The relationship between the dye structure and the lasing properties is studied in detail with the help of the photophysical and electrochemical properties as well as quantum mechanical simulations. The asymmetric substitution of the parent dye induces inhomogeneities in the charge distribution, which leads to an overall loss of the fluorescence capacity, mainly in polar media. Such non‐radiative deactivation processes can be softened by decreasing the electron‐donor ability of the substituent or even avoided by symmetrical substitution. Thus, grafting of the arylethyne moieties at the longitudinal axis of the indacene core results in an effective strategy to develop red‐edge BODIPYs with highly efficient and photostable laser emission.     

Conformations and steric and stacking interactions of trisubstituted ureas and thioureas with alkyl and phenyl groups

The monomeric ν(N—H) vibrations of various trisubstituted ureas of the R₂UPh type and -thioureas of the R₂TUPh type have been studied. The trans—out isomerism in the former and the trans—out—cis isomerism in the latter are discussed from the point of view of steric effect. The monomeric ν(N—H) vibrations of RPhUPh and RPhTUPh are also examined. The single band appearing in the spectrum of both ureas is characteristic of the cis form; this suggests the existence of phenyl—phenyl interaction (the stacking interaction proposed by Galabov et al. [10]). Behavior of ν(N—H) vibrations at several concentrations is shown to be clearly different in the three forms (trans, out and cis). The presence of the cis form is confirmed by solvent effect experiments.     

含茂基苯并三氮唑基镧系有机配合物的合成及表征

三茂基镧系化合物和苯并三氮唑在四氢呋喃中反应,合成了7个未见文献报道的含茂基苯并三氮唑基镧系有机配合物,经元素分析、IR和MS测定,从有关数据推测了这类配合物的可能结构。