流动注射在线共沉淀预富集火焰原子吸收法测定痕量铜

研究了以Ｎｉ＾２＋－ＤＤＴＣ为共沉淀载体，流动注射在线共沉淀预富集－火焰原子吸收光谱法测定痕量铜的体系，在０．３ｍｏｌ．Ｌ＾－１的硝酸介质中，铜离子在编织反应器中与Ｎｉ＾２＋－ＤＤＴＣ（产生共沉淀，并被收集在编织器内壁上，用甲基异丁基酮（ＭＩＢＫ）在线洗脱沉积物并引入火争原子化器中测定。当富集时间为４０ｓ时，４０μｇ．Ｌ＾－１的铜１０次测定的相对标准偏差为３．０％，灵敏度提高６０倍，检出限（３σ）     

MORPHOLOGICAL STUDIES OF PET FILMS WITH DIFFERENT CRYSTALLIZATION RATE IN DRAWING PROCESSES

Morphological changes during stretching of two PET samples (S and T) with different crystallization rate have been studied by means of SALS, solvent etching and polarizing microscope techniques. Results show that under the same drawing conditions larger and more perfect rod-like and spherulitic superstructures were formed more easily in the sample with higher crystallization rate (sample S). The amount of less compact regions which may be easily attacked by the vapor of allyl amine decreases more rapidly in sample S than in sample T during stretching, and these regions are more randomly distributed in sample T especially at low elongations. The difference of the two samples in morphological changes is coincident with their difference in tensile behavior.     

聚丙烯微孔膜基渐变聚合物的制备,结构与性能的研究

以聚丙烯微孔膜为基材，通过扩散控制原位共聚合的方法在人填充了组成沿膜的厚度方向逐渐改变的无规共聚物，Ｘ－光电子能谱（ＸＰＳ）、全反射红外光谱（ＡＴＲ）以及动态粘弹谱的分析结果。说明所制备得到的合膜具有明显的渐变聚合物性质。     

Liquid chromatography/electrospray tandem mass spectrometry method for the quantitation of fosinoprilat in human serum using automated 96-well solid-phase extraction for sample preparation

A sensitive, specific, accurate and reproducible liquid chromatography/electrospray tandem mass spectrometry method was developed and validated for the quantitation of fosinoprilat in 0.2 mL of human serum. The method employed acidification (with pH 4.0 sodium acetate buffer) of the serum samples to minimize the hydrolysis of the prodrug fosinopril to fosinoprilat prior to purification by automated 96-well solid-phase extraction. The required chromatographic separation of fosinoprilat and fosinopril was achieved isocratically on a Luna C8 analytical column (2 x 50 mm, 3 microm). The total run time was 2 min. The mobile phase contained methanol and water with 10 mM ammonium acetate. Detection was by positive ion electrospray tandem mass spectrometry. The standard curve, which ranged from 2.00 to 500 ng/mL, was fitted to a 1/x(2) weighted linear regression model. Fosinoprilat quality control (QC) samples used to determine the accuracy and precision of the method were prepared in human serum at concentrations of 5.00, 200, 400 and 1000 ng/mL. The assay accuracy was within 8% (dev). The intra- and inter-assay precisions were within 6 and 3% (RSD), respectively. Fosinopril QC samples used to gauge the rate of hydrolysis of fosinopril to fosinoprilat during the assay procedure were prepared in human serum at 500 ng/mL. The hydrolysis of fosinopril to fosinoprilat was 相似文献   

5—（4‘—溴—2’—羧基苯偶氮）罗丹宁与铜（Ⅱ）的显色反应及其应用

本报道了新显色剂５－（４’－溴－２’－羧基苯偶氮）罗丹宁的合成及在水溶液中的离解常数Ｋ１和Ｋ２，研究了该显色剂与铜（Ⅱ）的显色反应，在弱酸性时，试剂与铜（Ⅱ）形成摩尔比２：１的络合物，摩尔吸光系数为８．９×１０＾４Ｌ．ｍｏｌ＾－１．ｃｍ＾－１。当铜的浓度在０～２．７ｍｇ／Ｌ的范围内符合比耳定律。用分光光度法测定了合金中铜的含量。     

2,4,6—三氧—1,3,5,2—三氮磷杂环己烷衍生物的合成及其抗肿瘤活性

利用Ｎ，Ｎ－二（２－氯乙基）氨基磷酰二异氰酸酯和胺的加成反应，合成了２，４，６三氧－１，３，５，２三氮磷杂环己烷衍生物，它们的结构经＾１ＨＮＭＲ，ＩＲ和元素分析所证实。初步生物活性测试结果表明，部分化合物具有一定的抗肿瘤活性。     

Synthesis,crystal structure and magnetic properties of a series of polymeric lanthanoid–copper complexes [Ln2Cu3{O(CH2−CO2)2}6]·nH2O (Ln=La,Nd, n=9; Ln=Er,n=6)

The reaction of diglycolic acid, O(CH2CO2H)2, with Cu(NO3)2·2H2O and lanthanoid nitrate hydrate produces a series of novel Ln–Cu mixed metal complexes, [Ln2Cu3{O(CH2CO2)2}6]·nH2O (Ln=La, Nd, n=9; Ln=Er, n=6), which have been characterized by elemental analysis, i.r. spectroscopy, magnetic measurements and X-ray crystallography. The Ln3+ and Cu2+ ions are connected by the carboxylate groups of the ligands, resulting in the formation of a complicated network.     

超高效液相色谱-串联质谱法测定茶叶中游离氨基酸成分

建立了使用超高效液相色谱-串联质谱（UHPLC-MS/MS）高效、快速直接测定茶叶中游离氨基酸的方法。通过对质谱、色谱条件及氨基酸提取条件的优化，以含0.2%（体积分数）甲酸的5 mmol/L乙酸铵水溶液和甲醇为流动相进行梯度洗脱，在电喷雾离子（ESI）源正离子扫描模式下检测，通过UHPLC-MS/MS测定，共解析了茶叶中的20种氨基酸。结果表明，茶氨酸（Thea）、Arg、Asn和Asp在50~500 μg/L范围内线性关系良好，其他氨基酸在10~250 μg/L范围内线性关系良好，相关系数均大于0.99；加标回收率为92.3%~109.2%，相对标准偏差为2.00%~9.88%，检出限为0.001~0.011 mg/L，定量限为0.010~0.053 mg/L。该方法灵敏、准确，具有良好的重复性和稳定性，可有效检测出茶叶中的20种氨基酸及氨基类成分。     

Putting a brake on an autonomous DNA nanomotor

A strategy was developed to reversibly switch on/off an autonomous DNA nanomotor that contains a DNA enzyme. The multiple RNA cleavage of the DNAzyme powered the motor to move, and a strand displacement mechanism provided the basis for a reversible brake to the motor.     

A novel selective fluorescent chemosensor for Cu（Ⅱ）

A novel fluorescence enhancement Cu~(2 ) chemosensor derived from coumarin was prepared.Emission study found that it exhibits evident Cu~(2 )-amplified fluorescence prior to Co~(2 ),Pb~(2 ),Mg~(2 ),Mn~(2 ),Ni~(2 ),Zn~(2 ),Fe~(3 ),Ag~ and Cd~(2 ),and the largest emission enhancement factor is about 9 at a ratio of 2:1 (chemosensor 1/Cu~(2 )).