固相萃取毛细管气相色谱法测定卷烟滤嘴中7种挥发性羰基化合物

建立了SPE-GC测定卷烟滤嘴中7种挥发性羰基化合物,采用2,4-二硝基苯肼酸性溶液捕集滤嘴中挥发性羰基化合物,捕集液经Waters C18固相萃取小柱纯化和富集,用GC检测.7种羰基化合物检出限分别为0.02、 0.07、 0.04、 0.03、 0.03、 0.02、 0.03 μg/mL;回收率范围在92.0%～99.5%之间;相对标准偏差均小于5%.方法应用于国内5种烤烟型卷烟滤嘴的分析,得到理想结果.     

ZnHZSM-5上甲醇芳构化反应的研究

通过浸渍法改性制得ZnHZSM-5催化剂,并采用XRD、BET、NH₃-TPD和Py-IR方法对催化剂进行表征。在连续流动固定床反应装置上考察了Zn负载量和反应条件对甲醇芳构化反应(MTA)的影响。结果表明,0.5%Zn负载量可使芳烃收率提高5%。当Zn负载量超过2%时,不仅不能提高芳烃收率,反而促使甲醇裂解成CO和CO₂,Zn负载量为1.0%～2.0%时芳构化活性较高。最佳反应条件为液体体积空速0.36h^-1~0.6h^-1,温度350℃。并对Zn改性下的甲醇芳构化反应过程进行了探讨。     

超声波提取-气相色谱法测定土壤中21种酚类化合物

建立了超声波提取-气相色谱法同时测定土壤中21种酚类化合物的分析方法。用二氯甲烷和正己烷混合溶剂提取土壤中的酚类化合物,提取液经碱性水溶液分配净化,去除非酸性有机杂质,再酸化萃取酚类化合物,浓缩后采用气相色谱-氢火焰离子化检测器进行检测,外标法定量。以10 g土壤样品计,酚类化合物的检出限为0.01~0.06 mg/kg。实际样品添加回收试验的回收率为62.9%~111.4%,相对标准偏差为4.3%~24.0%(n=6),准确度和精密度均较好。结果表明:该法操作方便,净化效果好,可用于土壤中多种酚类化合物的测定。     

A Facile Synthesis of Indolizines by 1，3－Dipolar Cycloaddition of Pyridinium and Related Heteroaromatic Ylides with Alkenes in the Presence of TPCD，Py_4Co（HCrO_4）_2

ＡＦａｃｉｌｅＳｙｎｔｈｅｓｉｓｏｆｉｎｄｏｌｉｚｉｎｅｓｂｙ１，３－ＤｉｐｏｌａｒＣｙｃｌｏａｄｄｉｔｉｏｎｏｆＰｙｒｉｄｉｎｉｕｍａｎｄＲｅｌａｔｅｄＨｅｔｅｒｏａｒｏｍａｔｉｃＹｌｉｄｅｓｗｉｔｈＡｌｋｅｎｅｓｉｎｔｈｅＰｒｅｓｅｎｃｅｏｆＴＰ...     

聚乙烯载体催化剂的制备与表征

不同目数的聚乙烯粉末通过辐射方法接枝了4-乙烯基吡啶官能团.经甲基铝氧烷(MAO)预处理后负载了茂金属催化剂Cp₂ZrCl₂.光电子能谱和红外光谱结果表明催化剂通过MAO的作用负载在聚乙烯接枝4-乙烯基吡啶聚合物上.4-乙烯基吡啶的接枝含量、催化剂的负载率以及载体催化剂对乙烯单体的活性均随着聚乙烯粉末的颗粒减小而增大.     

单滴微萃取-气相色谱质谱联用法测定纺织品中可分解芳香胺

建立了单滴微萃取结合气相色谱-质谱法测定纺织品中可分解芳香胺的方法。研究了萃取剂种类、萃取剂体积、萃取时间、pH和搅拌速度等条件对单滴微萃取效率的影响。确定最佳萃取条件:在室温条件下,取5 mL样液,调节被萃取液pH8,以2μL氯苯为萃取剂萃取20 min,搅拌速度为200 r/min。在优化的实验条件下,检出限为0.08~0.14 mg/kg,线性范围0.5~50 mg/kg,线性相关系数大于0.996,平均加标回收率为75.3%~96.7%,相对标准偏差为3.6%~8.7%。方法适合纺织品中可分解芳香胺的测定。     

Extraction and Identification of Ginsenoside Re and Its Effects and Mechanism of Protecting Acute Renal Ischemia-reperfusion Injury in Rats

This paper studies the extraction and identification of ginsenoside Re from ginseng fruits and investigates the effect and mechanism of ginsenoside Re of protecting acute renal ischemia-reperfusion injury in rats.Having been smashed,the ginseng fruits were ultrasonically extracted twice with 95% ethanol for 30min each.Having been concentrated,the solution was dissolved with distilled water and separated by two-column chromatography,of which one was packed with macroporous resin D4020,and the other was packe...     

MALDI-TOF MS对难溶聚芳酰胺PA6T的分析表征

选用五种样品试剂三氟乙酸、四氢呋喃、甲酸、乙腈、60%乙腈/5%三氟乙酸和两种不同的制样方法,采用基质辅助激光解吸电离飞行时间质谱(MALDI-TOF MS)表征难溶性聚合物聚对苯二甲酸己二酰胺(PA6T)的结构和分子量。发现以60%乙腈/5%三氟乙酸为样品试剂所得谱图的分子质量范围和信噪比最大,且溶剂法一步点样优于无溶剂法制样。获得了离子液体中合成产物PA6T的链结构,表明其主链为线性,未发现环状聚合物的存在,存在三种端基结构聚合体： 两端均为氨基或羧基、或一端为氨基另一端为羧基。采用MALDI-TOF MS和SEC两种方法对比测量了PA6T的平均分子量和分子量分布指数,表明MALDI-OF MS测得的平均分子量低于SEC法,分子量分布指数也低于SEC法,这是由于MS处理数据时忽略了低分子量部分,且高分子量部分因难以离子化而无法得到引起的。对于难溶的聚芳酰胺类聚合物的结构和分子量及其分布表征,MALDI-TOF MS仍不失为一个好方法。     

杨氏模量实验仪器调节的一种优化方法及实施方案

指出杨氏模量实验调节的难点,用理论指导实践的方法分析调节困难的原因.并针对问题提出一种新的简单的调节方法--立靶法,有效地解决了瞄准难和调焦难的问题.还给出了立靶法的完整流程图,介绍了立靶法的实施方案.     

Differential Expression of Molecular Chaperones in PC12 Cells Treated with PSI

<正>Parkinson's disease(PD) is a common neurodegenerative disorder whose primary pathology features are the degeneration of dopaminergic neurons in the substantia nigra pars compacta(SNc) and the presence of eosinophilic inclusions called Lewy body in the cytoplasm of the remained neurons.Growing evidence suggests that dysfunction of the ubiquitin-proteasome system(UPS) is involved in the etiopathogenesis of PD.In order to investigate the pathogenetic mechanism of ubiquitin-proteasome dysfunction in PD,2D-differential gel electrophoresis (2D-DIGE) and MALDI-TOF Pro MS were used to determine the proteins,which were differentially expressed,in PC12 cells that had undergone a synthetic proteasomal inhibitor PSI(10μmol/L) treatment for 24 h.Forty-six protein spots were differentially expressed in response to PSI administration,of which 34 were increased and 12 decreased. Six of these were identified as molecular charperones:endoplasmin precursor(GRP94),heat shock protein 105(HSP105),HSC-70-psl,glucose ruglated protein 75(GRP75),glucose ruglated protein 58(GRP58) and heat shock 27000 protein 1(HSP27).The results suggest that the molecular chaperones play an important role in the PD model induced by proteasomal inhibitor.