SDE-GC-ECD分析水体中有机氯农药

运用单滴溶剂萃取-气相色谱-微池电子捕获检测器(SDE—GC—μECD)联用技术对水体中有机氯农药进行了分析，优化了影响单滴溶剂萃取的多种因素。该方法除了对P，P′-DDD的线性范围在0．4～4ng／mL之间外，其余的七种目标物(α-666，β-666，γ-666，δ-666，P，P′-DDE，0，P′-DDT，P，P′-DDT)线性范围均在0．04～4．0ng／mL之间，相关系数为0．9976～0．9999，回收率范围为83．3％～96．1％，相对标准偏差为2．1％～7．8％。与传统的液液萃取相比，单滴溶剂萃取不仅准确度、精密度相当，而且还具有省时、省溶剂的优点。     

Concentration and clean-up of trace hydrocarbons from atmospheric particulate matter

Summary The aim of this work is to establish the best conditions for concentration and purification steps in the trace analysis of aliphatic and polycyclic aromatic hydrocarbons (PAH) from atmospheric particulate matter by gas chromatography-flame ionisation detection (GC-FID) and high performance liquid chromatography with ultraviolet and fluorescence detection (HPLC-UV-FL). The best results for the more volatile compound were obtained with a combination of rotary evaporation and a stream of nitrogen (near to 100% for aliphatic hydrocarbons and from 70 to 105% for PAH). Two types of solid phase extraction (SPE)cartridges (Supelclean ^tm LC-Silica SPE tubes and Sep-Pak^? Plus silica cartridges) and glass column were examined for the purification and fractionation step. Blank chromatograms of both types of cartridges analysed by GC-FID made this study difficult, because a PSS (programmed split-splitless) injector was employed thereby increasing the sensitivity. This problem was not observed in the HPLC-UV-FL blank chromatograms of these cartridges. Glass columns filled with silica and alumina were chosen because no interference was found in the GC-FID blank chromatograms and the best recoveries in the fractionation of both aliphatic hydrocarbons and PAH were achieved. This is especially important when aliphatic hydrocarbons concentrations are lower than 1 μg mL⁻¹. Finally, the selected conditions were applied to the analysis of hydrocarbons in real atmospheric particulate samples.     

毛细管电泳中样品在线预富集方法

本文对高效毛细管电泳中样品在线预富集方法作了评述，包括瞬间等速电泳，反流速电泳，场放大进样，场放大排除基体和固相萃取等技术，引用文献81篇。     

A method for the determination of histamine in wine by HPLC with precolumn derivatization with phenylisothiocyanate

Summary A method for determining histamine in wine by precolumn derivatization with PITC (phenylisothiocyanate) with reversed-phase HPLC and UV detection is reported. Histamine can be determined together with the 24 amino acids within 40 min, or separately in a shorter time (less than 4 min) if a prior solid phase extraction clean-up is used.     

Use of capillary gas chromatography/sensory analysis as an additional tool for sampling technique comparison in peach aroma analysis

Capillary GC/sensory analysis was used to judge if dynamic headspace on sliced pulp and on intact fruit, and solvent extraction could collect the “character impact” and the “contributory” aroma compounds in peaches. Capillary GC/sensory data showed that the headspace techniques selectively recovered the “contributory” volatile compounds, which are strictly related to the characteristic odor of the various peach cultivars, whereas solvent extraction better quantified the “character impact” compounds (lactones).     

Chiral diphosphine ligands based on camphor: synthesis and applications in asymmetric hydrogenations

The synthesis of a novel class of atropisomer chiral diphosphine ligands with a bornene framework is described. The new ligands showed in Rh catalyzed asymmetric hydrogenation of α- and β-enamides very high ee’s (more than 99%).     

1,10-双(1′-苯基-3′-甲基-5′-氧代吡唑-4′-基)癸二酮-[1,10]与三苯基氧化膦对钐(Ⅲ)的协同萃取行为研究

研究了１，１０－双（１′－苯基－３′－甲基－５′－氧代吡唑－４－基）癸二酮－［１，１０］（ＢＰＭＰＤＤ，Ｈ２Ａ）与三苯基氧化膦（ＴＰＰＯ，Ｂ）的氯仿溶液从硝酸介质中对Ｓｍ（Ⅲ）的协同萃取行为，计算了体系的酸性协萃系数ＲＡ和协萃系数Ｒ，用斜率法测得协萃合物的组成为ＳｍＡ·ＨＡ·Ｂ，计算了协萃平衡常数，用萃取法制得了固态协萃合物，并对其组成、ＩＲ及ＴＧ－ＤＴＡ进行了研究     

Alkane oxygenation with H2O2 catalysed by FeCl3 and 2,2′-bipyridine

The H₂O₂-FeCl₃-bipy system in acetonitrile efficiently oxidises alkanes predominantly to alkyl hydroperoxides. Turnover numbers attain 400 after 1 h at 60 °C. It has been assumed that bipy facilitates proton abstraction from a H₂O₂ molecule coordinated to the iron ion (these reactions are stages in the catalytic cycle generating hydroxyl radicals from the hydrogen peroxide). Hydroxyl radicals then attack alkane molecules finally yielding the alkyl hydroperoxide.     

Determination of acetone, hexanal and heptanal in blood samples by derivatization with pentafluorobenzyl hydroxylamine followed by headspace single-drop microextraction and gas chromatography–mass spectrometry

In the study, we developed a simple, rapid, sensitive, and inexpensive method for determination of the disease biomarkers of acetone, hexanal and heptanal in human blood. For the first time, derivatization of carbonyls with O-2,3,4,5,6-(pentafluorobenzyl)hydroxylamine (PFBHA) was combined with headspace single-drop microextractin (HS-SDME) and gas chromatography-mass spectrometry (GC–MS) and applied to the analysis of acetone, hexanal, and heptanal in human blood. At first, acetone, hexanal and heptanal in blood were derivatized with PFBHA and formed oximes in several seconds. Sequentially, the oximes were headspace extracted and concentrated by a microdrop solvent. Finally, the extracted oximes were analyzed by GC–MS. HS-SDME conditions and method validations were studied. Due to needing of only 2 μl organic solvent, short extraction time of 8 min, and simple operation, derivatization-HS-SDME was shown to be a rapid, simple, and inexpensive technique for analysis of acetone, hexanal, and heptanal in human blood. Moreover, it had low detection limit values from 0.24 to 0.62 nM, and good reproducibility (R.S.D. less than 12%).     

锌盐及其化验研究

介绍了锌盐对人体的作用，对锌盐的化验方法进行了研究，包括锌的定性分析和定量分析。锌的定量分析又包括：EDTA滴定法和萃取吸光光度法。