使用疏水作用色谱研究蛋白质的构象变化

研究了高效疏水作用液相色谱中(HIC)色谱条件改变对蛋白质构象的影响。发现固定相配体的疏水性、温度及流动相中盐的阴离子、阳离子和pH值都影响蛋白质的构象。     

高效离子排斥色谱法测定饮料中的糖精钠

提出了一种用高效离子排斥色谱法测定饮料中糖精钠的新方法。以ＩｏｎＰａｃ ＩＣＥ－ＡＳ ６柱为分离柱，０．１０ ｍｍｏｌ／ＬＨ２ＳＯ４＋甲醇（９＋１）为淋洗液，２０２ｎｍ波长下紫外检测。在１－１００ｍｇ／Ｌ范围内，糖精钠的含量与峰面积呈 良好线性关系。检出限为０．６０ｎｇ，灵敏度优于以往采用离子交换色谱－电导检测法的结果。在实验条件下，饮料 中常见有机酸以及其它人工合成甜味剂等均不产生干扰。方法用于饮料中糖精钠的测定，加标回收率为９８％～ １０５％。此外还比较了电导检测、紫外检测和经化学抑制系统后紫外检测等三种检测方式对测定灵敏度的影响。     

环境水中甲基对硫磷、对硫磷和辛硫磷农药残留的SPE-HPLC分析

采用离线固相萃取 (SPE)富集 -高效液相色谱(HPLC)分离和紫外分光光度法检测 ,对环境水中甲基对硫磷、对硫磷和辛硫磷3种有机磷农药进行分析;固相萃取用C18 萃取柱 ,用甲醇洗脱 ,高效液相色谱分离以Shim_PackCLCODS柱(150mm×4.6mmid,5μm)为分离柱 ,流动相为甲醇 -水(体积比70∶30) ,紫外检测波长为280nm;该法稳定可靠 ,回收率高     

反相高效液相色谱法测定全血中马钱子碱和士的宁的含量

 建立了反相高效液相色谱法定量分析全血中马钱子碱和士的宁含量的方法。该方法应用Oasis  R ○ MCX固相萃取小柱进行提取、采用XTerra TM RP 18 色谱柱进行分离。在该条件下马钱子碱和士的宁的线性范围为0.05～10 mg/L ,最小检出限为0.15 ng。该方法测得马钱子碱和士的宁在低、中、高浓度下的回收率均在90%以上,日内、日间精密度均符合方法学要求。该方法灵敏、快速、准确,适用于临床血药浓度监测和法医毒化检验。     

高效液相色谱法分析蜂蜜中的糖

本文研究了用四乙撑五胺（简称ＴＥＰＡ）作为胺基改善剂，在硅胶柱上定量分析蜂蜜含糖量的方法，并成功地分离了木糖、果糖、葡萄糖、蔗糖、麦芽糖和乳糖。对操作条件进行了探讨。采用示差折光检测器检测，含０．０１％ＴＥＰＡ的乙腈－水（７７＋２３）作流动相。六种糖的相对标准偏差均小于３．５％。     

L-卡尼丁分子压印聚合物作为手性分离色谱固定相的研究

以L－卡尼丁为模板分子，分别以α－甲基丙烯酸和丙烯酰胺为功能单体，乙二醇二甲基丙烯酸酯为 剂，采用分子压印技术合成了对L－卡尼丁具有高选择性的分子压印聚合物。将所得聚合物用作高效液相色谱固定相，研究了它们对外消旋卡尼丁盐酸盐的拆分能力，分析结果表明，α－甲基丙烯酸作为功能单体所得聚合物对外消旋卡尼丁盐酸盐具有良好的拆分作用，其分离因子α为1．89。     

Studies on the Electrochemical Characteristics of K2FeO4 Electrode

Discharge performance of K2FeO4 electrode under different conditions was studied by the constant electric current discharge method. The electrochemical characteristics of K2FeO4 electrode were investigated for the first time by means of cyclic voltammetry. The results show that the K2FeO4 electrode made at moderate pressure (20MPa) and discharged at lower current has better discharge performance. It is also found that K2FeO4 electrode is significantly rechargeable.     

高效液相色谱法测定橡胶促进剂TBBS

采用反相高效液相色谱法（HPLC）测定了橡胶促进剂N－叔丁基－2－苯并噻唑次磺酰胺（TBBS）的纯度，标准偏差小于0．3。     

HPLC of synthetic polymers characterization of polystyrenes by high performance precipitation liquid chromatography (HPPLC)

Summary The advantages and disadvantages of high performance precipitation liquid chromatography have been demonstrated for polystyrene homopolymers. Depending on the mobile phase composition at the dissolution point of the polymeric sample and surface properties of the stationary phase, elution is governed either by a solution process or by adsorption. A contribution by adsorption was noticed on silica as well as on reversed phases based on silica with a normal phase gradient of increasing polarity (heptane to dichloromethane). Elution was solely governed by solubility of the polymers on both types of stationary phase for polystyrenes with a molecular weight above 35 000 and reversed phase gradient of decreasing polarity (methanol to dichloromethane). Under these conditions an identical dependence of elution solvent composition on sample size was found as for turbidity titrations. Due to differences in the velocity of the eluent front and the polymeric sample with porous stationary phases the polymers can be eluted as colloidal solutions Non-porous stationary phases are superior in this respect because the velocities of eluent and solutes are identical.     

QuEChERS/超高效液相色谱-串联质谱法同时测定水产品中四溴双酚A与六溴环十二烷

建立了同时测定水产品中四溴双酚A(TBBPA)和六溴环十二烷(HBCD)的超高效液相色谱-串联质谱方法。样品前处理采用QuEChERS方法,均质生物样品用水分散后加乙腈提取,经C_(18)分散固相萃取净化。采用CORTECS~?C_(18)色谱柱(4.6 mm×100 mm×2.7μm)分离,以甲醇-水为流动相进行梯度洗脱,流速为0.7 mL/min。采用电喷雾离子源,在负离子模式下以多反应监测(MRM)方式检测。结果表明,TBBPA和3种HBCD单体在0.5～500μg/L范围内线性良好,相关系数(r)大于0.998,检出限(LOD,S/N=3)和定量下限(LOQ,S/N=10)分别为0.04～0.16μg/kg和0.12～0.55μg/kg。在5、20、50μg/kg加标水平下的平均回收率为74.0%～121%,相对标准偏差(RSD)为0.20%～23%。该方法操作简单、快速、重现性好,适用于水产品中TBBPA和HBCD的快速检测。