引言北大核心CSCD

食品安全事关人民群众身体健康和生命安全,事关经济健康发展与社会和谐稳定。优异的分离分析技术是保障食品安全的重要手段,食品基质复杂,目标物种类繁多,且含量水平低,加之近年来食品安全有害物隐蔽性越来越强,通过化学性修饰等手段使目标物的形态多样等,给食品安全分离分析带来极大的挑战。     

Sulfamethazine and Sulfadimethoxine Separation Strategies Based on Molecularly Imprinted Adsorbents

Abstract

The synthesis of molecularly imprinted polymer (MIP) as a stationary phase of high‐performance liquid chromatography (HPLC), for the efficient determination of sulfamethazine and sulfadimethoxine in tablets is reported. The polymers were prepared by a noncovalent method with sulfamethazine as the template, methacrylic acid as the functional monomer and ethylene glycoldimethacrylate as the cross‐linker in the presence of chloroform as the solvent. The retention time of sulfamethazine and sulfadimethoxine were approximately 5.2±0.2 and 10.3±0.5 min, respectively. In order to compare the chromatographic data from the stationary phase, retention factor (k) and separation factors (α) were given. The values of α were 2.05～2.17 showed that the MIP was able to recognize structurally subtle differences from the template molecule.

The MIP was successfully applied to commercial tablet analysis and the result showed a good recovery with 99 and 98% for sulfamethazine and sulfadimethoxine.     

Separation of Chlorophylls and Their Degradation Products using Packed Column Supercritical Fluid Chromatography (SFC)

Complex mixtures of chlorophyll degradation products may arise during processing and storage of vegetable oil and green plant materials like broccoli and spinach. Determination of these compounds is important in the area of food chemistry. Therefore a method using packed column supercritical fluid chromatography (SFC) has been developed. The method comprises chromatography using a simple gradient of methanol in carbon dioxide at constant column back pressure of 30 MPa and a column temperature of 40°C. Effects of pressure and mobile phase composition showed the importance of applying a modifier gradient for optimal separation of the chlorophyll products. The method permits separation of 15 chlorophyll derivatives including chlorophyll a and b, pheophytins, and pyropheophytins on a C₁₈ column in about 20 minutes. Identifications of the individual peaks were based on reference compounds, the retention order of the compounds, and their absorption spectra.     

N-去甲万古霉素的亲和吸附

通过交联聚丙烯酸甲酯与乙醇胺反应,形成聚(N-羟乙基丙烯酰胺)树脂,在酸催化作用下与环氧氯丙烷反应,形成含有α-羟基氯乙基的树脂.含α-羟基氯乙基的树脂与D-丙氨酸、L-丙氨酸或甘氨酸反应,分别得到含有这3种氨基酸的吸附剂.这3种吸附剂吸附N-去甲万古霉素的结果表明,含D-丙氨酸的吸附剂的吸附量最大,含甘氨酸的吸附剂的吸附量次之,而含L-丙氨酸的吸附剂不吸附N-去万古霉素.说明前两种吸附剂对N-去甲万古霉素存在亲和吸附作用.含D-丙氨酸吸附剂的最佳吸附pH值为5.8,当吸附液中的盐(NaCl)浓度增加时,吸附量降低.用0.4mol/LNa₂CO₃/CH₃CN(摩尔比7∶3,pH=9.5)作为洗脱剂可完全脱附被吸附的N-去甲万古霉素.     

血液净化高分子吸附材料

简要总结了我们近年来在血液净化高分子吸附材料方面取得的研究成果. 对于有机小分子吸附剂、中分子吸附剂和生物大分子吸附剂的系统研究,不仅取得了大量的基础性研究结果,而且筛选出了性能优良的血液净化吸附剂,已经与血液灌流装置一起开始应用于临床.     

Selection of A Suitable Solvent System for the Separation and Quantitation of Histamine

Abstract

The suitability of 79:21, 85:15 and, 90:10 of phosphate buffer: 50% methanol, as mobile phases, to separate and quantitate histamine in small plasma volume (<300 μl) was investigated by using a Dionex BioLC System coupled to a pulsed amperometric detector. Also, special attempts were made to reduce the time of analysis of each sample. Methylhistamine was used as an internal standard. the best results were obtained with the 79:21 mobile phase with concommittant reduction in analysis time from the current 1 sample per 90 min to 5 samples per 60 min suggesting that the method is suitable and cost effective.     

Differences in the Efficiency of Separation of Analgesic Drugs by High-Performance Thin-Layer Chromatography with Similar Octadecyl Silica-Based Adsorbents

JPC – Journal of Planar Chromatography – Modern TLC -     

Extraction and Separation Properties of Hydrophilic Compounds Using Novel Water-Holding Adsorbents Bonded with a Zwitter-Ionic Polymer

A novel water-holding adsorbent was synthesized by introducing a zwitter-ionic polymer to a hydrophilic methacrylate base resin. The retention abilities of the hydrophilic compounds on the adsorbents with and without cross-link in the zwitter-ionic functional groups were examined. The amount of held water on the non-cross-linked adsorbent was higher than that of the cross-linked one. The extraction efficiencies of the hydrophilic solutes on the adsorbents were evaluated by the solid phase extraction method. These adsorbents showed high affinity for nucleosides and glycosides, and good recoveries for such hydrophilic compounds in the solid-phase extraction were obtained. Furthermore, the retention properties of the hydrophilic solutes on the adsorbents were also evaluated by LC. The hydrophilic solutes were retained on these adsorbents by a partition mode based on a hydrophilic interaction. The retention factors of the hydrophilic solutes showed good correlation to their log P _o/w (logarithm of octanol?Cwater partition coefficient) and good separation based on hydrophilic interaction was obtained for nucleobases and nucleosides.     

Titania-Based Adsorbents for Hydrophilic Interaction Liquid Chromatography

Journal of Analytical Chemistry - Stationary phases based on titania are obtained by the adsorptive attachment of polyethyleneimine followed by crosslinking with 1,4-butanediol diglycidyl ether....     

Cyclic Tetramers of Zinc Chlorophylls as a Coupled Light‐Harvesting Antenna–Charge‐Separation System

A coupled light‐harvesting antenna–charge‐separation system, consisting of self‐assembled zinc chlorophyll derivatives that incorporate an electron‐accepting unit, is reported. The cyclic tetramers that incorporated an electron acceptor were constructed by the co‐assembly of a pyridine‐appended zinc chlorophyll derivative, ZnPy , and a zinc chlorophyll derivative further decorated with a fullerene unit, ZnPyC₆₀ . Comprehensive steady‐state and time‐resolved spectroscopic studies were conducted for the individual tetramers of ZnPy and ZnPyC₆₀ as well as their co‐tetramers. Intra‐assembly singlet energy transfer was confirmed by singlet–singlet annihilation in the ZnPy tetramer. Electron transfer from the singlet chlorin unit to the fullerene unit was clearly demonstrated by the transient absorption of the fullerene radical anion in the ZnPyC₆₀ tetramer. Finally, with the co‐tetramer, a coupled light‐harvesting and charge‐separation system with practically 100 % quantum efficiency was demonstrated.     

以壳聚糖为载体的内毒素吸附剂

内毒素血症(Endotoxemia)可出现于多种疾病过程中,导致器官坏死、不可逆休克和死亡。如何及时并有效地清除患者体内的内毒素,是临床医学面临的一个难题．选用高效吸附剂,籍助血液灌流的方法从血液中直接清除内毒素,受到了人们越来越多的关注。     

寡肽吸附剂的制备及吸附机理

为清除尿毒症患者血清中分离出的八肽VVRGCTWW(V8), 制备了不同间隔臂长含苯环的吸附剂Phenc. 吸附实验结果显示, 吸附剂Phe3c具有非常好的吸附能力. 采用NMR和分子模拟技术对吸附剂的模型体系的吸附机理进行了研究. 结果显示, 配体中的苯环可与八肽形成π-π堆积, 而且间隔臂的增长可以克服空间位阻效应, 有效增加配体与V8的作用几率, 进而增强吸附剂与八肽的相互作用. 研究结果表明, 采用合理的分子模型及分子对接方法, 不仅可以合理解释吸附剂的吸附机理, 而且可用于吸附剂的虚拟筛选.     

计算机模拟内毒素吸附剂吸附机理的研究

应用计算机模拟的方法研究了内毒素吸附剂的吸附机理. 模拟结果显示, 以二甲胺为配体的吸附剂, 当β位存在羟基时, 此羟基可与内毒素分子间形成氢键, 并形成一个八元环的稳定结构. 此时吸附剂与内毒素之间存在静电、 氢键、 疏水相互作用和八元环的协同作用. 同时模拟了羟基位于配体不同位置的吸附剂与内毒素的相互作用. 结果表明, 静电作用为主要的相互作用力, 羟基的位置对吸附剂的吸附能力影响显著.     

Structure of Porous Adsorbents

Porous solids are gaining in importance as adsorbents and catalysts both for scientific investigations and for industrial applications. Adsorbents having predetermined pore structure can be prepared by specific synthesis. This pore structure can be described in detail and comprehensively by specific parameters, which can be determined by gas adsorption measurements and by other means. Information concerning the bonding state and the concentration of the functional groups on the surface is obtainable by the use of chemical and physical methods of investigation. Other functional groups can be attached to the surface by chemical reactions. It is possible in this way to prepare selective adsorbents.     

Adsorption-Induced Deformation of Adsorbents

Adsorption-induced deformation of AR-V and AUK carbon adsorbents and NaX zeolite has been studied upon adsorption of n-С₅Н₁₂, n-С₆Н₁₈, n-С₇Н₁₆, and CO₂ at temperatures of 193?423 K. It has been shown that adsorption-induced deformation is positive upon the physical adsorption of gases and vapors on the surface of a nonporous (macroporous) solid when the excess adsorption is positive. When calculating the adsorption-induced deformation in the region of the capillary-condensation filling of mesopores, the additional pressure in capillaries, which is negative (contraction of an adsorbent), must be taken into account in the case of wetting a solid surface with a liquid adsorbate. The compressibility of AUK microporous carbon adsorbent as a porous solid is almost independent of the temperature and the properties of an adsorbate, and, for adsorption of n-C₅H₁₀ and n-C₇H₁₆ hydrocarbons and CO₂, it is γ_а = (5.6 ± 0.6) × 10^?6 bar^?1. The compressibility of AUK adsorbent appears to be 87% higher than that of nonporous graphite.     

N-去甲万古霉素亲和吸附剂的合成及性能

将N,N二甲基丙烯酰胺N,N′乙撑双丙烯酰胺共聚物部分水解,在共聚物中引入适量的羧基.含羧基的聚合物与氨基酸甲酯缩合,然后使酯基皂化,将氨基酸引入聚合物.将革兰氏阳性菌细胞壁粘肽的三种类似物(-Gly,-Gly-DAla,-Gly-DAla-DAla)分别引入上述聚合物,合成了3种万古霉素系列抗菌素的亲和吸附剂(Ⅰ,Ⅱ和Ⅲ).结果表明,吸附剂Ⅱ和吸附剂Ⅲ对N去甲万古霉素的吸附量分别为0.80和0.86mmol/g;最佳吸附pH值为6左右;吸附剂Ⅰ的吸附量随着吸附液中盐浓度的增加而显著降低,而吸附液中盐浓度对吸附剂Ⅱ的吸附量影响较小.说明亲和作用在吸附剂Ⅱ的吸附中贡献较大.用0.4mol/LNa₂CO₃(pH9.5)/CH₃CN(体积比为7/3)作为洗脱剂可完全脱附被吸附的N去甲万古霉素.     

Correction to: Differences in the Efficiency of Separation of Analgesic Drugs by High-Performance Thin-Layer Chromatography with Similar Octadecyl Silica-Based Adsorbents

JPC – Journal of Planar Chromatography – Modern TLC -     

二维相关分析中参考谱的选择对分离重叠峰的影响

二维相关光谱是一项将光谱强度看作两个独立的光谱变量的函数的技术, 它是由动态光谱经过数学转化后得到的. 在扰动过程中, 动态光谱等于实际测得的光谱减去参考谱, 参考谱的选择是任意的, 甚至可以为0, 但是在实际应用时, 人们逐渐发现参考谱的选择会对二维相关光谱产生一定的影响. 本篇文章采用模拟的方法, 建立光谱模型, 光谱强度按e指数形式单调变化, 比较以平均谱为参考谱和不设参考谱得到的二维相关光谱图, 分析它们的区别, 在不同参考谱条件下, 利用二维相关光谱分离重叠峰, 得到的结果也不相同, 将两种条件综合利用可以得到更多更正确的信息.     

A Pitfall in Heavy Metal Separation with Amino-modified Silica Adsorbents from Aqueous Solution: The Occurring pH Shift

Selective separation of heavy metal ions from acidic aqueous solutions is of strong interest for certain industrial processes, such as electroplating, as well as environmental protection, for example battery recycling. Amino-functionalized adsorbents are often discussed as suitable material for this purpose. Herein, two silica-based adsorbents functionalized with 3-aminopropyl- and 3-[2-[2-aminoethylamino]-ethylamino]-propyl-ligands resulting in adsorbents MonoA and TriA, respectively, were investigated regarding their separation behavior with focus on nickel(II) and cobalt(II) in batch as well as continuous flow experiments in acidic aqueous solutions. For both adsorbents, pH shifts into the alkaline range were observed in the process solutions, causing precipitation of metal hydroxides mainly in the particle pores in case of adsorbent MonoA and a combination of precipitation and adsorption regarding adsorbent TriA. Contrary to prior studies, our findings evidence that amino-functionalized adsorbents are not applicable for nickel(II) and cobalt(II) in selective adsorption processes and additionally demonstrate that, besides batch investigations, continuous flow experiments are essential for well-founded adsorbent selections in process development.