海藻酸钠-壳聚糖-桑椹红微囊的制备

以海藻酸钠-壳聚糖为复合囊材采用锐孔法制备桑椹红微囊,探讨了海藻酸钠浓度、壳聚糖浓度、Ca Cl2浓度、桑椹红浓度、针头孔径、下滴高度、温度、转速等因素对微囊包封率的影响。确定了最佳制备工艺条件为海藻酸钠浓度4.0%、壳聚糖浓度2.5%、氯化钙浓度2.0%、桑椹红浓度0.50%、针头孔径0.390mm、下滴高度4cm、温度为20℃、转速为300r·min-1。制得的微囊药物含量为11.28%,包封率为88.93%。     

基于制备接枝型分子印迹膜构建农药电位型电化学传感器及其检测性能研究

基于分子设计,以氯甲基化聚砜(CMPSF)为基膜,阴离子单体对苯乙烯磺酸钠(SSS)为功能单体,N,N'-亚甲基双丙烯酰胺(MBA)为交联剂,在表面引发体系-NH2/S2O2-8的作用下,采用"接枝聚合与分子印迹同步进行"的分子表面印迹新技术,制备了接枝型农药抗蚜威分子印迹膜(MIM)。采用红外光谱(FITR)和光学显微镜(OM)对该分子印迹膜进行表征,通过等温结合实验与竞争吸附实验,考察了抗蚜威分子印迹膜的分子识别性能与机理。以该印迹膜作为敏感膜,构建了抗蚜威电位型传感器,并对其检测性能进行了考察。结果表明,所制备的接枝型印迹膜对模板抗蚜威分子具有特异的识别选择性和优良的结合亲和性,结合容量高达92μg/cm2,相对于分子结构与抗蚜威相似的阿特拉津,印迹膜对抗蚜威的选择性系数为4.537。在p H 4.0的水介质中,传感器膜电极的电位响应与抗蚜威浓度对数在1.0×10-6~1.0×10-3mol/L范围内呈良好的线性关系(r=0.999 9),其检出限为2.5×10-8mol/L;以抗蚜威分子印迹膜为敏感膜所构建的电位型传感器,其构建过程简捷,检测灵敏准确,电位响应快速(t10 s)。     

亚硫酸氢钠-过氧化氢超微弱化学发光体系用于核黄素检测

亚硫酸氢钠(Na HSO3)和过氧化氢(H2O2)反应可产生微弱的化学发光。核黄素对亚硫酸氢钠和过氧化氢的化学发光有极大的增强作用,且化学发光强度在0.02~2.0μg/m L范围内与核黄素浓度呈良好的线性关系。据此,建立了核黄素的高灵敏化学发光分析方法,方法检出限为0.007μg/m L,相对标准偏差(n=11)不大于1.6%。利用荧光光谱、化学发光谱对核黄素增强Na HSO3-H2O2体系化学发光的机理进行探讨,为该体系的应用研究提供了新思路。     

邻菲啰啉-Fe(Ⅱ)分光光度法测定头孢唑啉钠

建立了用邻菲啰啉-Fe(Ⅱ)分光光度法测定头孢唑啉钠的方法 .头孢唑啉钠在0.10mol·L-1 NaOH溶液中,100℃水浴加热降解为含巯基的化合物.巯基化合物把Fe3+还原为Fe2+.加入邻菲啰啉显色,通过测定生成的橘红色配位化合物的吸光度间接测定头孢唑啉钠的含量.头孢唑啉钠浓度在0.02~40mg·L-1范围内呈现良好线性关系,线性回归方程A=0.043c(mg·L-1)-0.001,相关系数R=0.998 8,表观摩尔吸光系数ε=2.05×104 L·(mol·cm)-1,相对标准偏差RSD=1.27%,检测限(3σ/k)0.065mg·L-1.在此基础上,测定了市售头孢唑啉钠粉针剂的含量,回收率在99.17%~101.2%之间,结果令人满意.     

液相色谱串联质谱法测定水果中复硝酚钠残留量

以甲醇提取样品,采用超高效液相色谱串联质谱法(UPLC–MS/MS)测定水果中复硝酚钠的残留量。以甲醇–10 mmol/L乙酸铵水溶液(体积比为60∶40)为流动相,质谱采用电喷雾负离子MRM检测模式。对硝基苯酚钠和5-硝基愈创木酚钠的线性范围为0.05~2.00 mg/L,检出限为0.01 mg/kg,邻硝基苯酚钠的线性范围为2.5~100.0 mg/L,检出限为0.5 mg/kg,线性相关系数均大于0.995。实际样品中对硝基苯酚钠、邻硝基苯酚钠和5-硝基愈创木酚钠的加标回收率分别为83.0%~93.4%,81.0%~87.4%,83.0%~91.8%,测定结果的相对标准偏差小于7%(n=6)。该法操作简单、快捷,精密度、准确度高,适用于水果中复硝酚钠的残留分析。     

Iron–Oxalato Framework with One‐Dimensional Open Channels for Electrochemical Sodium‐Ion Intercalation

Discovery of a new class of ion intercalation compounds is highly desirable due to its relevance to various electrochemical devices, such as batteries. Herein, we present a new iron–oxalato open framework, which showed reversible Na⁺ intercalation/extraction. The hydrothermally synthesized K₄Na₂[Fe(C₂O₄)₂]₃ ? 2 H₂O possesses one‐dimensional open channels in the oxalato‐bridged network, providing ion accessibility up to two Na⁺ per the formula unit. The detailed studies on the structural and electronic states revealed that the framework exhibited a solid solution state almost entirely during Na⁺ intercalation/extraction associated with the reversible redox of Fe. The present work demonstrates possibilities of the oxalato frameworks as tunable and robust ion intercalation electrode materials for various device applications.     

芳香寡聚磺酸酯桥联大环化合物的合成及其对Sn2+和Bi3+的识别作用

以4,6-二烷氧基-1,3-苯二磺酰氯和芳香二酚为原料,三乙胺作缚酸剂,二氯甲烷作溶剂,采取一步成环法合成了3种磺酸酯桥联大环化合物。合成产物的结构用IR、¹H NMR、¹³C NMR和MALDI-TOF等技术手段进行了确认。利用紫外光谱分析的方法研究了4,6,16,18-四正戊氧基-11,23-二甲基-1,3,13,15-四磺酸酯间苯芳香大环(5)对Ca²⁺、Pb²⁺及部分过渡金属等20种金属离子的识别。结果发现,其对Sn²⁺显示出一定的选择性,由于Sn²⁺和Bi³⁺协同作用的影响,在化合物5-Sn²⁺的体系中加入Bi³⁺,紫外吸收光谱在325 nm左右的吸收增强了许多,这说明化合物5对Bi³⁺显示出优于Sn²⁺的较好选择性。     

Structure and further fragmentation of significant [a3 + Na − H]+ ions from sodium‐cationized peptides

A good understanding of gas‐phase fragmentation chemistry of peptides is important for accurate protein identification. Additional product ions obtained by sodiated peptides can provide useful sequence information supplementary to protonated peptides and improve protein identification. In this work, we first demonstrate that the sodiated a₃ ions are abundant in the tandem mass spectra of sodium‐cationized peptides although observations of a₃ ions have rarely been reported in protonated peptides. Quantum chemical calculations combined with tandem mass spectrometry are used to investigate this phenomenon by using a model tetrapeptide GGAG. Our results reveal that the most stable [a₃ + Na ? H]⁺ ion is present as a bidentate linear structure in which the sodium cation coordinates to the two backbone carbonyl oxygen atoms. Due to structural inflexibility, further fragmentation of the [a₃ + Na ? H]⁺ ion needs to overcome several relatively high energetic barriers to form [b₂ + Na ? H]⁺ ion with a diketopiperazine structure. As a result, low abundance of [b₂ + Na ? H]⁺ ion is detected at relatively high collision energy. In addition, our computational data also indicate that the common oxazolone pathway to generate [b₂ + Na ? H]⁺ from the [a₃ + Na ? H]⁺ ion is unlikely. The present work provides a mechanistic insight into how a sodium ion affects the fragmentation behaviors of peptides. Copyright © 2015 John Wiley & Sons, Ltd.     

Preyssler heteropolyacid supported on silica coated NiFe2O4 nanoparticles for the catalytic synthesis of bis(dihydropyrimidinone)benzene and 3,4-dihydropyrimidin-2(1H)-ones

A novel magnetic acidic catalyst comprising Preyssler (H14[NaP5W30O110]) heteropoly acid support‐ed on silica coated nickel ferrite nanoparticles (NiFe2O4@SiO2) was prepared. The catalyst was character...     

A High‐Voltage and Ultralong‐Life Sodium Full Cell for Stationary Energy Storage

Recently, there has been great interest in developing advanced sodium‐ion batteries for large‐scale application. Most efforts have concentrated on the search for high‐performance electrode materials only in sodium half‐cells. Research on sodium full cells for practical application has encountered many problems, such as insufficient cycles with rapid capacity decay, low safety, and low operating voltage. Herein, we present a layered P2‐Na_0.66Ni_0.17Co_0.17Ti_0.66O₂, as both an anode (ca. 0.69 V versus Na⁺/Na) and as a high‐voltage cathode (ca. 3.74 V versus Na⁺/Na). The full cell based on this bipolar electrode exhibits well‐defined voltage plateaus near 3.10 V, which is the highest average voltage in the symmetric cells. It also shows the longest cycle life (75.9 % capacity retention after 1000 cycles) in all sodium full cells, a usable capacity of 92 mAh g^?1, and superior rate capability (65 mAh g^?1 at a high rate of 2C).