基于光谱自编码微球的多样品免疫荧光混合筛选和荧光成像

研究了微球粒度、温度、pH和包被液浓度对聚苯乙烯微球免疫吸附的影响。将20种编码微球与20个样品对映包被,进行免疫荧光混合筛选,分析荧光信号最强微球的光谱编码,确定了阳性样品的编号。其异硫氰酸荧光素(FITC)荧光标记抗体筛选灵敏度可达体积稀释比1∶2000。采用氩离子激光扫描荧光成像技术,成功实现了基于光谱自编码微球的多样品免疫荧光混合筛选和荧光成像。     

量子点-聚苯乙烯复合微球的制备及荧光光谱的研究

用无皂乳液聚合制备了交联聚苯乙烯微球,讨论了单体、引发剂浓度,共聚单体等对微球粒径,单分散性的影响,并用FTIR和SEM对上述样品的结构进行了表征。在单体的配方中,加入1%二乙烯基苯作为交联剂,加入1%丙烯酸使小球表面功能化,便于后续与无机量子点和有机材料的结合。以氯仿/正丁醇为混合溶胀剂,将聚合物微球与CdSe量子点或CdSe/ZnS复合,制得含有两种或两种以上的不同量子点的高分子复合荧光微球。通过荧光光谱的测试,出现了两个或两种以上互不干扰的特征峰。为在聚合物微球中注入多种量子点,制得荧光探针,并实施量子点编码进行了初步的前期探索工作。     

核-壳结构二氧化硅介孔材料的制备与表征

采用溶胶凝胶法在一定条件下合成了具有核-壳结构的二氧化硅介孔材料,使用透射电子显微镜对微球样品的超微结构进行了观察,使用傅里叶红外光谱分析了样品的光谱性质。分析结果表明:制备的核-壳结构介孔二氧化硅微球样品,是由外表面为孔径约8纳米,厚度约30纳米的有序介孔二氧化硅壳层,包裹着内核为直径约200纳米的二氧化硅微球所组成,介孔壳层具有较大的比表面积,具有良好的光谱性质。     

羧基化磁性微球固定化谷氨酸脱羧酶

通过化学共沉淀法结合高锰酸钾氧化制备羧基化Fe_3O_4磁性微球,以该磁性微球作为载体,固定化谷氨酸脱羧酶。利用热重分析(TGA)、透射电镜(TEM)及振动样品磁强计(VSM)对羧基化磁性微球进行表征,结果表明该磁性微球磁含量约为95.1%,粒径均一,呈近似球形且具有超顺磁性。通过对固定化酶进行傅里叶红外光谱(FT-IR)、VSM和X射线衍射(XRD)分析,确定磁性微球载体与谷氨酸脱羧酶分子间形成酰胺键,实现共价结合且固定化酶前后粒子晶形完整,均具有良好的磁响应能力和超顺磁性。与游离谷氨酸脱羧酶相比,固定化酶的热稳定性和酸碱耐受性均有不同程度的提高,且制备的固定化酶重复使用10批后相对酶活力仍大于90%。     

羧基化磁性微球固定化谷氨酸脱羧酶

通过化学共沉淀法结合高锰酸钾氧化制备羧基化Fe₃O₄磁性微球，以该磁性微球作为载体，固定化谷氨酸脱羧酶。利用热重分析（TGA（、透射电镜（TEM（及振动样品磁强计（VSM（对羧基化磁性微球进行表征，结果表明该磁性微球磁含量约为95.1%，粒径均一，呈近似球形且具有超顺磁性。通过对固定化酶进行傅里叶红外光谱（FT-IR（、VSM和X射线衍射（XRD（分析，确定磁性微球载体与谷氨酸脱羧酶分子间形成酰胺键，实现共价结合且固定化酶前后粒子晶形完整，均具有良好的磁响应能力和超顺磁性。与游离谷氨酸脱羧酶相比，固定化酶的热稳定性和酸碱耐受性均有不同程度的提高，且制备的固定化酶重复使用10批后相对酶活力仍大于90%。     

静电喷雾法制备超细CL-20基复合含能微球及其性能研究

为了使六硝基六氮杂异伍兹烷(CL-20)球形化并且降低其反应活化能,采用静电喷雾法成功制备了超细NC/CL-20复合含能微球。通过控制静电喷雾实验条件及前驱体溶液参量,得到了球形度完整、粒径在1~3μm且粒度分布较窄的复合物微球颗粒,并且探究了CL-20含量对微球粒度的影响;对该复合微球进行了红外光谱分析、X射线衍射分析、热分解反应动力学研究。结果表明,复合微球中CL-20与NC之间仅为物理复合;原料CL-20为ε晶型,而静电喷雾制备的复合微球中CL-20均为β晶型;几种复合微球的放热峰温均低于原料CL-20;NC/CL-20复合微球的分解反应活化能比原料CL-20降低了28.47kJ/mol。     

溶胀法制备高强度聚苯乙烯荧光及编码微球

通过对荧光微球制备的传统溶胀法的改进,以二氯甲烷作溶胀剂,0.25%SDS水溶液作分散体系(促进疏水性染料溶胀进入种子微球以增加微球荧光强度),制备出了荧光强度高,单分散性好(平均粒径3.6μm,变异系数3.7%),光学性质稳定,定量染色的绿色、橙色、红色三种荧光微球。将发生荧光共振能量转移的两种染料同时溶胀进种子微球中,制备了能产生双荧光信号的荧光编码微球。     

犬粪便中细粒棘球绦虫抗原双抗体夹心ELISA检测方法的建立及应用

目的建立简便、特异的检测犬粪便中细粒棘球绦虫抗原的双抗体夹心ELISA方法,并进行验证及初步应用。方法以细粒棘球绦虫EdiagA864蛋白为抗原,免疫日本大耳白兔,制备多克隆抗体;利用HRP标记兔抗细粒棘球绦虫EdiagA864多克隆抗体,通过溶解、超声方法处理犬粪便样品;以抗细粒棘球绦虫单克隆抗体2D12作为捕获抗体,HRP标记的兔抗细粒棘球绦虫EdiagA864多克隆抗体为检测抗体,通过棋盘法确定抗体最佳包被浓度、最佳封闭剂、待检粪样最佳稀释比例及酶标抗体最佳浓度。应用建立的双抗体夹心ELISA法对来自长春地区的64份犬粪便样品及来自新疆的8份犬粪便阳性样品进行检测。结果兔抗EdiagA864多克隆抗体的效价为105。建立的双抗体夹心ELISA法的最佳检测条件为:抗体包被浓度为1∶50,封闭剂为1%BSA,粪液稀释度为1∶5,酶标二抗稀释度为1∶800。建立的双抗体夹心ELISA法与犬贾第虫和犬蛔虫阳性样品均无交叉反应;检测不同稀释度的粪便液,当稀释至1∶20时,P/N仍大于2;检测6份阳性样品与4份阴性样品的批间和批内变异系数均小于8。用建立的方法检测8份阳性样品的结果均为阳性,64份待检样品的结果均为阴性。结论建立的双抗夹心ELISA方法特异性较强,敏感性较高,重复性较好,为细粒棘球绦虫流行病学调查及诊断提供了一种更简便、快速、特异的免疫学检测方法。     

壳聚糖/卵磷脂复合微球固定木瓜蛋白酶的研究

以壳聚糖和卵磷脂为材料,采用乳化-交联法制备壳聚糖/卵磷脂复合微球,并用光学显微镜和红外光谱对微球进行表征;再以此微球作为载体固定木瓜蛋白酶,以固定率为指标,应用正交试验法优选固定化酶的制备工艺,并对固定化酶的半衰期、米氏常数(Km)、操作稳定性进行研究.结果表明,制备的壳聚糖/卵磷脂复合微球呈完整的圆球形或椭球形;固定化酶的优化制备工艺为:m(壳聚糖)=250 mg,m(壳聚糖):m(卵磷脂)=1:2,V(戊二醛水溶液)=300 μL,m(木瓜蛋白酶)=20 mg,此时制备的固定化酶的固定率达61.94％,半衰期为86.27 h,米氏常数为6.37 mg/mL,固定化酶有很好的操作稳定性.     

Ag_3PO_4/BiOBr光催化剂的制备与可见光活性研究

先采用水热法制备具有分等级结构的BiOBr微球,然后采用沉积-沉淀法将Ag3PO4负载于BiOBr微球表面。采用扫描电子显微镜、X-射线粉末衍射仪、N2吸脱附等温线和紫外-可见漫反射光谱对所制备的样品进行了测试表征;将Ag3PO4/BiOBr微球用于可见光催化分解甲基橙溶液,考察了Ag3PO4的负载量及重复使用对可见光(420nm)催化活性影响的研究。结果表明:Ag3PO4/BiOBr微球具有分等级介孔-大孔结构,Ag3PO4与载体BiOBr间结合紧密。单纯BiOBr微球几乎没有可见光催化活性,负载Ag3PO4后表现出较好的可见光催化活性,其中以Ag3PO4(50%)/BiOBr样品的催化效果最佳,30min内将近90%的甲基橙被降解,该催化剂样品在重复实验中表现出较好光催化稳定性。     

Preparation of slow release encapsulated insecticide and fertilizer based on superabsorbent polysaccharide microbeads

The use of encapsulated fertilizers and pesticides is a key approach for slowing the release of agrochemicals, while simultaneously reducing costs and environmental problems. The use of hybrid systems for encapsulation in organic-based agriculture, which enables the release of agrochemicals in a single application, has been a growing field. In this approach, a formulation of Bacillus-thuringiensis as bio-pesticide and nitrogen, phosphorus, and potassium fertilizer (fish emulsion, potassium nitrate, and potassium phosphate) were formulated using superabsorbent polymers microbeads based on sodium alginate (ALG) then evaluated for release. Different formulations were prepared using 15 wt% of Bt, fish emulsion, nitrogen, and phosphorus. The encapsulated microbeads were prepared by wet-extrusion processing using sodium alginate as the superabsorbent polymer and calcium chloride as the gelling agent. The resulting beads were characterized in terms of size, morphology, water uptake, and biodegradability. The results showed that the prepared microbeads have narrow size distributions (1.2 to 2.1 mm) and increased water uptake (1,200–3,200%). Moreover, loaded microbeads were analyzed using inductively coupled plasma-optical emission spectroscopy and Elementar CHNS analyzer to obtain the fertilizer grades as (6.2–0.8–1.05), (0–6.3–6.4), and (0.62–0–2.4) for the one loaded with fish emulsion, for potassium phosphate loaded beads, and for potassium nitrate loaded beads, respectively.     

Shaping of alumina microbeads by drop-casting of the photopolymerizable suspension into silicone oil and UV curing

The alumina microbeads were obtained by forming the drops of alumina suspensions in a silicone oil followed by UV curing. Due to the strong hydrophobic properties, silicon oil is a non-solvent (non-miscible) to the suspensions, thus the formation of perfectly rounded beads occurs spontaneously. The size of beads was controlled by a selection of a needle diameter and the position of needle tip: above or immersed in silicone oil. Thanks to that it was possible to obtain beads with diameters from 1000 to 1300 µm. The obtained alumina microbeads were characterized by quite a narrow size distribution, the differences in the size of the beads, within one series, did not exceed 1.5%. The research showed that the higher alumina volume fraction in suspensions favors the development of microstructure and thus influences mechanical properties. It was proved that the application of the methyl silicone oil as the environment responsible for the formation of the beads does not affect the sintering process.     

湖北枣阳郭家庙曾国墓地出土"石英珠"(釉砂)的测试分析及其制作工艺模拟实验分析

运用显微观察、X射线衍射物相分析、X射线荧光分析成分测试和烧成实验等手段,对湖北枣阳郭家庙曾国墓地出土＂石英珠＂（釉砂）胎体及表面釉层进行了分析,以研究其烧制工艺。结果表明：这些＂石英珠＂是选用粉碎过的纯石英作原料,掺和少量黏合剂等塑型后,表面施以低铁的黏土与石灰或草木灰及含铜着色物混合配制的釉料（类似原始瓷的上釉工艺）,置于窑炉中烧制而成的釉砂;实验模拟了其可能的制作工艺。     

Preparation and characterization of manganese, nickel and cobalt ferrites submicron particles in sulfonated crosslinked networks

Magnetic submicron particles of MnFe₂O₄, NiFe₂O₄ or CoFe₂O₄ were created in or around the porous sulfonated beads based on poly(styrene-co-divinylbenzene) using an in situ inorganic precipitation procedure. The copolymer beads were treated with a mixed iron/cobalt chloride electrolyte and the doped copolymer networks were converted to their oxides by reaction with sodium hydroxide and potassium nitrate in aqueous solution. Energy dispersive X-ray spectroscopy (EDS) coupled to scanning electron microscopy (SEM) allowed the observation of the presence of submicron particles in the 0.1-0.5 μm size range, which chemical microanalysis of emitted X-rays revealed the presence of metal oxide particle, such as nickel, manganese or cobalt iron oxide. The morphological features of the binary material particles have depended on the ferrite type. All beads have presented dispersed and agglomerated submicron particles of ferrite located on their surface and inner part as well. Magnetization data of the microbeads showed good ferromagnetic behavior.     

CoPcS/TiO_2/beads及TiO_2/beads光催化降解水面漂浮植物油

以钛酸四丁酯为原料,以空心玻璃微珠为载体,采用溶胶-凝胶法制备出TiO2/beads光催化剂,用浸渍法制备出CoPcS/TiO2/beads光催化剂。研究了TiO2/beads及CoPcS/TiO2/beads光催化降解水面漂浮植物油的最优条件。结果表明,酸性或中性条件下,375 W中压汞灯照射2~3 h,TiO2/beads与CoPcS/TiO2/beads的投加量分别为3 g与1 g时,植物油的去除率达90%以上,投加微量的H2O2,可大大提高两者的光催化去除率。     

中间相沥青微球的活化

用KOH为活化剂,在不同活化条件下对中间相青微球进行活化,制备出比表面积为3182m^2/g,总孔容为2．45mL/g,苯吸附值为1320mg/g的高比表面积活性炭微球。研究了了KOH配比、活性温度和活化时间对活性炭微球的收率、比表面积和苯吸附值的影响。研究表明：随着KOH配比量或活化温度的提高,活化收率下降,活性炭微球的比表面积和七吸附值升高到一定值后下降;延长活化时间使活化反应进行完全,活性炭微球的活化收率、比表面积和苯吸附值仅有轻微变化。     

GDX203色谱固定相的改性及在羰基合成醋酸中的应用

甲醇羰基化反应制醋酸,是一个重要的化学反应[1],无论在实验室或在工业生产上,其反应过程的监测均是以色谱为分析手段[2,3]。由于该反应产物的组分多(甲醇、水、碘甲烷、乙酸甲酯、醋酸),通常采用色谱程序升温的方法才可达到各组分的分离[4],这种方法由于存在分析周期长和由于反应物在色谱柱中的保留时间长而发生变化影响了定量的准确性的缺点,给对该反应进行的快速、准确的监测带来诸多不便。     

Tailoring thermoresponsive microbeads in supercritical carbon dioxide for biomedical applications

The preparation of smart polymeric particles in supercritical carbon dioxide (scCO₂) presents many advantages for biomedical applications over conventional processes due to the easy elimination of trace contaminants rendering highly pure particles. Herein we report the successful optimization of poly(N-isopropylacrylamide) (PNIPAAm) synthesis strategy to obtain cell-sized hydrogel microbeads with defined and systematically varied mechanical properties. The effect of using different hydrophilic cross-linkers such as N,N-methylenebisacrylamide (MBAm), di(ethylene) glycol dimethacrylate (DEGDMA) and glycerol dimethacrylate (GDMA), on beads morphological, physico-chemical and mechanical properties was investigated. In agreement with a larger water uptake ability beads cross-linked with DEGDMA are more compliant than those containing MBAm or GDMA, having lower stiffness as accessed through oscillatory measurements on a rotational rheometer. Cytotoxicity assays showed that the obtained cross-linked PNIPAAm microbeads do not present any toxic effect on fibroblast cell cultures. Microbeads biocompatibility and adequate mechanical compliance enable their potential application on biomedical settings.     

Cu(II)‐incorporated,histidine‐containing,magnetic‐metal‐complexing beads as specific sorbents for the metal chelate affinity of albumin

N‐Methacryloyl‐(L )‐histidine methyl ester (MAH) was synthesized from metharyloyl chloride and histidine. Spherical beads with an average size of 150–250 μm were obtained by the suspension polymerization of ethylene glycol dimethacrylate and MAH in an aqueous dispersion medium. Magnetic poly(ethylene glycol dimethacrylate‐co‐N‐Methacryloyl‐(L )‐histidine methyl ester) [m‐p(EGDMA‐co‐MAH)] microbeads were characterized with swelling tests, electron spin resonance, elemental analysis, and scanning electron microscopy. The specific surface area of the beads was 80.1 m²/g. m‐p(EGDMA‐co‐MAH) microbeads with a swelling ratio of 40.2% and 43.9 μmol of MAH/g were used for the adsorption of bovine serum albumin (BSA) in a batch system. The Cu(II) concentration was 4.1 μmol/g. The adsorption capacity of BSA on the Cu(II)‐incorporated beads was 19.2 mg of BSA/g. The BSA adsorption first increased with the BSA concentration and then reached a plateau, which was about 19.2 mg of BSA/g. The maximum adsorption was observed at pH 5.0, which was the isoelectric point of BSA. The BSA adsorption increased with decreasing temperature, and the maximum adsorption was achieved at 4°C. High desorption ratios (>90% of the adsorbed BSA) were achieved with 1.0M NaSCN (pH 8.0) in 30 min. The nonspecific adsorption of BSA onto the m‐p(EGDMA‐co‐MAH) beads was negligible. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 93: 2669–2677, 2004