Detection of metalloproteins in human liver cytosol by synchrotron radiation X-ray fluorescence combined with gel filtration chromatography and isoelectric focusing separation

Synchrotron radiation X-ray fluorescence (SRXRF) spectroscopy is an advanced method of quantitative multielemental analysis with space resolution of several microm and sensitivities in the microg g(-1) range. It can be used for keeping track of trace elements after an electrophoretic separation of biological samples. In this paper, proteins in human liver cytosol were separated with gel filtration chromatography and thin layer isoelectric focusing (IEF). The contents of metal ions in protein bands were determined by SRXRF. The results showed that in the molecular weight (MW) range of 10 approximately 25 kDa, there were at least 2 Zn-containing bands with isoelectric point (pI) of 5 approximately 6 and 6.2 approximately 7, respectively and about 11 Fe-containing proteins with pI of 4.4, 4.6, 4.8, 5.0, 5.2, 5.3, 5.5, 5.6, 6.6, 6.8, and 7.2, respectively, present in human liver cytosol. The Zn-containing band with pI of 5-6 is the dominant species of zinc in this MW range. In addition, the Cu-containing bands with pI of 5.0 and below 4.8 were also detected. It is demonstrated that the procedure could be widely used in further investigations of the chemical species of trace elements in biological samples.     

SYNTHESIS OF A HYPERBRANCHED POLYETHER EPOXY THROUGH ONE- STEP PROTON TRANSFER POLYMERIZATION AND ITS APPLICATION AS A TOUGHENER FOR EPOXY RESIN DGEBA

A novel liquid hyperbranched polyether epoxy（HBPEE）based on commercially available hydroquinone（HQ）and 1,1,1-trihydroxymethylpropane triglycidyl ether（TMPGE）was synthesized through an A₂ + B₃ one-step proton transfer polymerization.In order to improve the toughness,the synthesized HBPEE was mixed with diglycidyl ether of bisphenol A （DGEBA）in different ratios to form hybrids and cured with triethylenetetramine（TETA）.Thermal and mechanical properties of the cured hybrids were evaluated.Results show that addition of HBPEE can improve the toughness of cured hybrids remarkably at < 20 wt%loading,without compromising the tensile strength.However,the glass transition temperature（T_g）of the cured hybrids decreases with increasing HBPEE content.Fracture surface images from scanning electron microscope show oriented fibrils in hybrids containing HBPEE.The formation and orientation of the fibrils can absorb energy under impact and lead to an improvement of toughness.Furthermore,based on the morphology of fractured surfaces and the single T_g in each hybrid,no sign of phase separation was found in the cured hybrid systems.As a result,the toughening mechanism could be explained by in situ homogeneous toughening mechanism rather than phase separation mechanism.     

Separation of strontium from associated elements with selective specific resin and extraction chromatography

In this paper,separation of Sr from associated elements（Na,K,Ca,Mg,and Ba） was carried out using an extraction chromatographic column packed with Sr selective specific resin consisting of an octanol solution of 4,4’（5’）-bis（t-butylcyclohexo）-18-crown-6 sorbed on an inert polymeric support.Using 8.0 mol/L HNO₃ as the eluent,Ba and associated elements were eluted immediately from the column, whereas Sr was strongly retained.The adsorbed Sr could then be stripped from the column as the eluent was changed to 0.05 mol/L HNO₃.Complete Sr/Ba separation was demonstrated to be feasible in that Ba could be washed from the column leaving pure Sr by adequate rinsing with 8.0 mol/L HNO₃. Furthermore,matrix effect could be effectively eliminated and the selectivity of the method was improved.The method was applied for the determination of Sr in the high purity barium carbonate （BaCO₃） product and seawater.The recoveries of Sr in 2 samples were determined to be 93.2%and 109%, respectively.     

A convenient phosphoryloxylactonization of pentenoic acids with(diacetoxyiodo)benzene

<正>The convenient one-pot method for phosphoryloxylactonization of alkenoic acids was reported:when(diacetoxyiodo)benzene, various 4-pentenoic acids and phosphates were mixed in CH_3CN at room temperature,phosphoryloxylactones were obtained in good to excellent yields in short times,some had two diastereoisomers.