Influence of clay on the morphology and phase separation behavior of poly(methyl methacrylate)/poly(styrene-co-acrylonitrile) blends

The effect of clay on the morphology and phase-separation behavior of poly(methyl methacrylate)/poly(styreneco-acrylonitrile)(PMMA/SAN) blends and the variation of clay dispersion have been investigated. With the evolution of phase separation in PMMA/SAN, most of the clays are first located at the boundaries between PMMA and SAN, and then gradually move to the PMMA-rich domain, owing to the affinity of clay to PMMA. The introduction of clay causes the increase of binodal and spinodal temperatures of PMMA/SAN and enlarges their metastable region, indicating the phase stabilizing effect of clay on the matrix. But the influence of clay on the cloud points obviously depends on the composition of PMMA/SAN. The selective adsorption of PMMA on the clay results in the difference between the composition of surface layer and that of polymer matrix. Hence, the clay plays the role of an agent changing the conditions of phase structure formation.     

冷冻去脂-液液分配净化/气相色谱-质谱法测定化妆品中16种多环芳烃

建立了保湿护肤系列化妆品中16种多环芳烃的气相色谱-质谱测定法。对于水剂样品,采用环己烷提取、浓缩等简单前处理;对于膏霜剂样品,采用乙腈+丙酮(8+2,V/V)涡旋提取样品中的待测物,提取液经冷冻去脂、液液萃取净化(氨水-环己烷、水-环己烷),气相色谱-质谱法测定。16种多环芳烃在1～50μg/L均与对应峰面积呈良好线性关系。添加量在1～50μg/kg时,平均回收率(n=6)为78.1%～103.7%,相对标准偏差为2.4%～7.1%,方法检测限为1～10μg/kg。该法可用于化妆品中16种多环芳烃的测定。     

黄原脂棉富集-电感耦合等离子质谱法测定海水中的重金属元素

采用黄原脂棉富集技术,建立了电感耦合等离子质谱法测定海水中重金属Cu,Pb,Zn,Co,Cd含量的方法。完善前处理条件,优化仪器工作参数,选取Rh,Ir作为内标元素,有效克服基体效应及仪器波动影响。Cu,Pb,Zn,Co,Cd的检出限分别为1.26,0.21,0.24,0.0027,0.0051μg/L,RSD为0.77%~3.3%,回收率为87.2%~96.0%。方法适用于海水中重金属元素的含量测定。     

花青醛的合成工艺优化

以3-异丙基苯乙酮(1)为原料,经3步反应合成了花青醛[3-(3-异丙基苯基)丁醛(4)],并优化了反应条件。确定合成3-(3-异丙基苯基)-2-丁烯酸乙酯(2)的最优条件为：n(1)/n(磷酰基乙酸三乙酯)/n(氢化钠)=5/6/6,于室温反应12 h,收率84.5%;合成3-(3-异丙基苯基)-1-丁醇(3)的最佳条件为:n(2)/n(硼氢化钠)/n(六水合二氯化钴)/n(二异丙基胺)=10/20/1/2,于55 ℃反应24 h,收率87.8%;合成4的最优条件为: n(3)/n(乙酸酐)/n(亚硝酸钠)=5/4/15,投料顺序为:乙酸酐、3、亚硝酸钠,反应时间为2 min,收率91.0%。产物结构经¹H NMR, ¹³C NMR和MS(ESI)确证。     

论海量存储在数字图书馆中的地位及模式选择

论述了海量存储在数字图书馆发展中的必然性,通过对目前流行的3种海量存储方式的比较,指出了各馆在进行海量存储方式选择时的一些建议。     

Synthesis and Primary Research on Antitumor Activity of Three New Panaxadiol Fatty Acid Esters

For making use of Ginseng resources that exhibit an antitumor activity and for finding new anticancer drugs,three new fatty acid ester compounds: 3β-acetoxy panaxadiol ( Ⅰ ), 3β-palmitic acid aceloxy panaxadiol ( Ⅱ ), and 3β-octadecanoic acid aceloxy panaxadiol( Ⅰ , Ⅱ , and Ⅲ ) were synthesized with panaxadiol, diacetyl oxide, palmityl chloride and stearyl chloride, and their structures were determined via MS, 13C NMR, IR, TLC, and so on. The molar yields of the three compounds are 75.14%, 79. 08%, and 72. 57%, respectively. Meanwhile, the antitumor activity of the three new panaxadiol fatty acid ester derivatives and panaxadiol was compared by using the method of MTT. Tumor cell used was Vero cell line. Positive control was 5-FU, blank was an RPMI1640 culture medium, negative control was an RPMI1640 culture medium and the solvent for drugs to be tested. Compound Ⅰ has the strongest antitumor activity followed by panaxadiol; compounds Ⅱ and Ⅲ have similar and weakest antitumor activities.Furthermore, the antitumor activities of the panaxadiol fatty acid ester derivatives show positive correlation with the concentration of the test group, but show no relationship with the molecular weight of fatty acid. The methods that are used to synthesize the three compounds with high yields and strong antitumor activities are simple and show a great potential for meeting the needs of industrial manufacture of these drugs.     

电感耦合等离子体-原子发射光谱法测定CPU导热硅脂中的铅和镉

采用几种消解方法对样品进行前处理,建立了电感耦合等离子体-原子发射光谱法(ICP-AES)同时测定导热硅脂中铅、镉等有害金属元素的方法.结果表明:高温灰化法Pb、Cd有损失;(1 1)王水湿法消解法Pb有损失;硝酸-高氯酸湿法消解法Pb和Cd几乎无损失;该方法精密度范围为0.22%-2.40%,Pb和Cd检出限分别为0.030μg·mL-1和0.006μg·mL-1.与石墨炉原子吸收光谱法(GFAAS)相比,ICP-AES具有简单、快速、准确等特点.     

自动电位滴定法测定SAN混合液中叔十二碳硫醇(TDM)的含量

采用万通自动电位滴定仪测定SAN混合液中TDM含量,通过实验确定乙醇代替异丙醇,支持电解液从100mL降至50mL进行实验是可行的,降低了检验成本。     

基于液质联用技术对早期高脂血症金黄地鼠肝脏鞘脂的靶向代谢组学研究

目的 对高脂血症金黄地鼠肝匀浆中鞘脂进行相对定量的靶向代谢组学研究.方法 18只SPF级叙利亚金黄地鼠随机分为正常对照组和高脂血症模型组,饲喂6周后进行血液生化检测,取肝脏进行HE染色,观察两组动物血液生化指标和组织病理学变化.基于液质联用技术,采用主成分分析(PCA)和偏最小二乘法分析(PLS-DA)进行模式识别,对...