固相萃取-超高效液相色谱-电喷雾串联质谱法同时测定烤鱼中15种杂环胺含量

建立了固相萃取-超高效液相色谱-电喷雾串联质谱同时分析烤鱼中15种杂环胺(HAs)含量的方法.样品经甲醇-1.0 mol/L NaOH均质、涡旋振荡、超声提取,采用 Licbrolut EN固相萃取柱净化,用乙醇-二氯甲烷溶液洗脱,收集洗脱液,水浴下用氮气吹干,加入乙酸-乙酸铵缓冲液涡旋溶解,以乙腈定容,微孔滤膜过滤,...     

超高效液相色谱-四极杆飞行时间串联质谱法同时分析奶粉中9种雌激素

建立了奶粉中9种雌激素(雌三醇、β-雌二醇、α-雌二醇、马烯雌甾酮、17α-乙炔雌二醇、雌酮、己烯雌酚、己二烯雌酚、己烷雌酚)的超高效液相色谱-四极杆飞行时间串联质谱(UPLC-Q-TOF-MS)分析方法.样品用水溶解,乙腈超声提取雌激素,正己烷除脂,NH2柱净化,经Waters ACQUITY UPLC HSS T3...     

轮烷类化合物的合成方法研究进展

轮烷类互锁分子因其多样的结构和性质,多年来一直是超分子化学领域的一个热点.综述了近年来轮烷类化合物的合成及制备方法,包括用传统的模板法(引入氢键、疏水作用、静电效应、配位和离子诱导等超分子作用)制备轮烷类化合物.除此之外,还介绍了利用“Click”化学、“穿线-收缩”、“穿线-膨胀”、自排序组织和自由基识别等新的合成手段来制备这类化合物.     

超高效液相色谱-串联质谱快速筛查葡萄酒中的14种禁用食品添加剂

建立了同时测定葡萄酒中14种禁用食品添加剂的超高效液相色谱-电喷雾电离串联质谱(UPLC-ESI-MS/MS)分析方法。采用UPLC BEH C18(100 mm×2.1 mm×1.7 mm)色谱柱,对流动相的组成、缓冲液离子强度及质谱的各种参数进行了优化。结果表明,流动相的离子强度对食品添加剂的质谱检测有重要影响,以含1 mmol/L甲酸铵-甲酸缓冲液(pH 3.9)-乙腈为流动相,梯度洗脱,柱温35℃,可以在6 min内完成14种食品添加剂的分离和检测。在ESI负离子模式下,采用选择离子监测方法进行测定时,除三氯蔗糖、日落黄和酸性红13的检出限分别为10,2和2 mg/L外,其它11种的检出限在0.01~1.0 mg/L之间。回收率为93.8%~106%,相对标准偏差小于3.1%。本方法快速、准确、灵敏度高,可用于葡萄酒及其它复杂基质食品中的低剂量、多种禁用食品添加剂的同时筛查。     

聚合物功能化纳米探针用于肿瘤坏死因子(TNF-α)的超灵敏检测

肿瘤坏死因子(TNF-α)是免疫系统中细胞所产生的一种重要炎症因子,广泛参与到一些自身免疫疾病的病理损伤过程中。在健康人体内,TNF-α浓度非常低,而在病患者体内则会发生成倍的增长。TNF-α的过度表达会导致一些慢性炎症的病发,如风湿性关节炎、牛皮癣等,同时它还与败血性休克综合症、糖尿病等疾病的发生存在关联,因而是癌症和感染疾病在发病初期的     

雄激素非依赖前列腺癌细胞系代谢组学的初步研究

探讨雄激素依赖性前列腺癌LNCaP细胞系向雄激素非依赖性前列腺癌细胞系(LNCaP-AI和LNCaP-AI+F)转变过程的代谢组学变化,寻找前列腺癌发生雄激素耐药的可能发生机制.利用超高效液相色谱-四极杆-飞行时间质谱,在电喷雾电离源在正离子模式下,采用60%(V/V)甲醇-0.85%(w/V)NH4HCO3溶液在-4...     

Hydrothermal Synthesis and Crystal Structure of a Novel Hexanuclear Copper（Ⅱ） Complex：[Cu_6（DPPZ）_4（btc）_4（H_2O）_8]·5H_2O

A new hexanuclear copper(Ⅱ) complex,[Cu 6 (DPPZ) 4 (btc) 4 (H 2 O) 8 ]·5H 2 O (1,DPPZ=dipyrido[3,2-a:2,3-c]phenazine,H 3 btc=1,3,5-benzenetricarboxylic acid),has been hydrothermally synthesized and structurally characterized by X-ray single-crystal diffraction,elemental analyses,IR,and thermogravimetric analysis.Its crystal structure is of triclinic system,space group P1 with a=12.489(4),b=14.234(5),c=14.484(5),α=82.848(4),β=79.399(4),γ=73.646(4)°,V=2421.2(13) 3,Z=1,Cu 6 C 108 H 78 N 16 O 37,M r=2573.17,D c=1.752 g/cm 3,μ=1.398 mm-1,F(000)=1308,GOOF=1.011,the final R=0.0495 and wR=0.1030 for 5420 observed reflections with I > 2σ(Ⅰ).In 1,four btc 3ligands act as bridges between six neighboring Cu atoms to form an unusual hexanuclear copper cluster.The clusters are further connected by two types of O-H···O and O-H···N hydrogen bonds,generating a three-dimensional supramolecular structure.In addition,intermolecular and intramolecular π-π stacking interactions further consolidate the three-dimensional supramolecular framework of 1.     

Synthesis and Crystal Structure of（2E,6E）-2,6-bis（2,3-dimethoxybenzylidene）cyclohexanone

The new title compound (2E,6E)-2,6-bis(2,3-dimethoxybenzylidene)cyclohexanone (C 24 H 26 O 5,M r=394.45) has been synthesized,and its crystal structure was studied.The title compound crystallizes in the orthorhombic system,space group Pca2 1 with a=17.536(2),b=14.8515(16),c=8.0512(9),V=2096.8(4) 3,Z=4,D c=1.250 g/cm 3,λ=0.71073,μ=0.087 mm-1 and F(000)=840.The structure was solved by direct methods and refined to R=0.0533 and wR=0.1248 from 2727 observed reflections (I > 2σ(Ⅰ)).The title molecules are connected through hydrogen bonds to generate a 3-D supramolecule.The preliminary biological tests showed definitely biological activity for the title compound.     

多级孔WO3/ZrO2固体酸催化剂的制备与表征

采用复合模板表面活性剂辅助水热法一步合成了WO3/ZrO2多级孔固体酸催化剂,并应用X射线衍射、低温N2吸附-脱附、拉曼光谱及NH3程序升温脱附对催化剂进行了表征.结果表明,WO3的引入使得WO3/ZrO2催化剂的比表面积增大,表面的酸中心明显增加.在乙酸和正丁醇的酯化反应中,WO3/ZrO2多级孔固体酸催化剂表现出较...     

Syntheses, Crystal Structures and Properties of Two Supramolecules Assembled from Weak Interactions

Two complexes, [Cu2(Htdb)4(H2O)2] (1) and [Cd(bipy)2(Hmcmbc)2] (2) (H2tdb = 2,2-thiodibenzoic acid, H2mcmbc = m-(carboxyl-methyloxy)-benzenecarboxylic acid, bipy = 4,4'-bipyridine), have been prepared, and were characterized by elemental analysis, FT-IR and single-crystal X-ray diffraction. Structures indicate that complex 1 is a single molecule, and 2 is a one-dimensional chain. Their two-and three-dimensional frameworks are constructed through hydrogen bonding, π…π or C–H…π stacking, and such other weak interactions. The cyclic voltametric behavior of complex 1 and luminescence property of complex 2 were investigated. 1 belongs to the triclinic system, space group P with a = 7.8607(6), b = 11.7619(9), c = 15.3481(12) , α = 109.3670(10), β = 92.4420(10), γ = 92.0450(10)°, V = 1335.65(18) 3, Mr = 1256.26, Dc = 1.5619(2) g/cm3, F(000) = 642, μ = 1.029 mm–1, Z = 1, the final R = 0.0289 and wR = 0.0763 for 5199 observed reflections with I > 2σ(I). Complex 2 crystallizes in triclinic, space group P with a = 9.6378(10), b = 9.7508(10), c = 19.055(2) , α = 88.7020(10), β = 80.5260(10), γ = 69.2000(10)o, V = 1649.9(3) 3, Mr = 815.07, Dc = 1.641 g/cm3, μ = 0.732 mm-1, F(000) = 828, Z = 2, the final R = 0.0511 and wR = 0.1149 for 4729 observed reflections (I > 2σ(I)).