Elimination of matrix effects for headspace solid-phase microextraction of important volatile compounds in red wine using a novel coating

In this paper, hydroxy-terminated silicone oil-butyl methacrylate-divinylbenzene (OH-TSO-BMA-DVB) copolymer was first synthesized and used as stationary phase with the aid of γ-methacryloxypropyltrimethoxylsilane (KH-570) as bridge in solid-phase microextraction (SPME) using sol–gel method and cross-linking technique. It has high extraction efficiency for both polar alcohols and fatty acids and nonpolar esters in comparison with commercial PDMS, PDMS-DVB and PA fibers. A simple and sensitive headspace SPME-gas chromatography (HS-SPME-GC) method using the novel fiber was presented for the simultaneous analysis of both polar alcohols and fatty acids and nonpolar esters in wine. To check the matrix effects, various model wine matrices, including distilled water; 11.5% ethanol/water (v/v) solution; a concentrated synthetic wine; a ‘volatile-free’ wine and a real wine were investigated in detail. Matrix effects were compensated for by using internal standard method and selecting the ‘volatile-free’ wine as working standard. The method presented in this study showed satisfactory linearity, precision, detection limits and accuracy. The recoveries obtained ranged from 85.87 to 104.2%, and the relative standard deviation values were below 9%. The results obtained indicated that the present method is a validated and accurate procedure for the simultaneous determination of both polar and nonpolar aroma compounds in wine.     

掺C60有机玻璃的吸收光谱研究

研究了Ｃ６０分别在有机玻璃（ＰＭＭＡ）和正己烷中的吸收光谱，发现Ｃ６０在有机玻璃中的吸收峰同在正己烷中相互对应，同时前者的吸收峰相对于后者峰宽变大，峰位产生红移，分析了产生这种现象的原因。     

毛细管电泳安培检测扑热息痛及其水解物

研究了各种电化学预处理条件下碳纤维电极对扑热息痛及水解物的电化学行为。确定该体系最佳预处理条件为０．２Ｖ电位下阳极化１ｍｉｎ，再于－２．０Ｖ下阴极化１０ｓ。预处理后的碳纤维伏安响应得到明显提高。运用最佳条件并在支持电解中加入添加剂后，扑热息痛及其水解物在毛细管电泳上获得很好的分离和检测。其中扑热息痛的检测下限为２．７８ｐｇ；对氨基酚为１．８４ｐｇ。     

流通池介质交换差示脉冲阳极溶出伏安法用于多元素重叠峰的分离及其同时测定

本文用流通池介质交换差示脉冲阳极溶出伏安法在盐酸介质中富集,而以碳酸钠-碳酸氢钠缓冲溶液为溶出介质,有效地分离了酸性介质中Cu(Ⅱ)、Sb(Ⅲ)、Pb(Ⅱ)、Tl(Ⅰ)、Cd(Ⅱ)、In(Ⅲ)的重叠溶出峰,实现了多离子的同时测定。     

纸基质室温燐光法测定痕量核黄素的研究

本文以国产滤纸为基质,醋酸汞作重原子微扰剂,详细研究了 RTP 的各种条件,成功地建立了测定核黄素的纸基质室温燐光法(PS-RTP)。结果表明,核黄素标准曲线线性范围为5×10~(-6)～1×10~(-3)mol/L,检出限为0.75ng。将该法用于血清中核黄素的测定,标准回收率在93.5％～103％之间。     

LaNi4Fe催化合成氨反应性能的研究

用冶金法、还原扩散法、共沉淀法制得了LaNiFe,并对其催化合成氨反应性能进行了研究。实验结果表明:还原扩散法,共沉淀法制得的LaNi_4Fe催化活性均比冶金法好。X—射线分析指出LaNi_4Fe在合成氨反应过程中变为Ni_4Fe和LaN。     

A Two-dimensional Lanthanide Coordination Framework with a New Amide-type Tripodal Ligand, 2,2′,2＂-Nitrilotris{[（2′- benzylaminoformyl）phenoxy]ethyl}amine

The La(III) complex with a new amide‐type tripodal ligand,2,2′.2″‐nitrilotris{[(2′‐benzylaminofomyl)‐phenoxylethyl)amine (L), was synthesized and characterized by X‐ray crystallographic analysis. Crystal data: C₄₈H_55.50LaN₇O_18.75, M_r=1169.40, monoclinic. space group, P2₁/n, a= 1.0644(3) nm. b=2.3889(5) nm, c= 2.1917(5) nm, β=90.65°, V=5.573(2) nm³, Z=1, D_c=1.394 g°cm^?3, R₁=0.0487, wR [1>2s?(I)]=0.1266. The results reveal that each La(III) ion binds to 9 oxygen atoms, three of which belong to carbonyl groups from three tripodal ligands and six to three bidentate nitrate groups and a two‐dimensional sheet of 4.8² networks is assembled by metal‐ligand coordination interaction. L, a heptadentate compound, merely acts as a tridentate bridging spacer due to its steric hindrance and links the La(III) ions as three‐connected nodes.     

因子分析—伏安法同时测定波峰重叠的混合物组份

本文将目标因子分析用于伏安分析法同时测定波峰重叠的混合物组份。用此法对Ｐｂ（Ⅱ）、Ｔｌ（Ｉ）混合体系的导数脉冲伏安重叠峰数据进行解析，获得了较理想的结果。