拟多维高效液相色谱法分离纯化双峰驼精清中的活性蛋白

利用一种新的高效液相色谱洗脱技术，建立了 ｐＨ缓冲液／离子对二元洗脱模式，对双峰驼精清的两种提取物的反相柱上进行了分离，得到了较纯的活性蛋白组分。该法操作简单、快速、比常规ＨＰＬＣ有更高的选择性及峰容量，并可减少活性蛋白的失活。     

基于遗传算法优化的约束背景双线性分解算法用于改进高效液相色谱灰色分析体系的校正结果

该文采用约束背景双线性分解算法(CBBL)对以高效液相色谱(HPLC)方法分离分析的灰色分析体系进行了多元校正研究。针对采用包括CBBL在内的矩阵校正方法处理HPLC灰色分析体系的固有缺陷,即在相关组分的色谱保留时间重现性较低的情形下多元校正的结果不理想,对CBBL方法进行了改进,即将待测组分的浓度与组分的色谱保留时间同时作为优化的参量引入CBBL,并采用遗传算法(GA)优化CBBL,对于模拟的组分保留时间飘移严重的HPLC灰色分析体系及保留时间重现性不佳的多种酚类化合物组成的实际HPLC灰色分析体系进行了多元校正分析,成功克服了经典CBBL的固有缺陷,取得了较理想的多元校正结果。另外,该研究所建议的方法的校正结果也显著优于传统的残差双线性分解法(RBL)以及秩消失因子分析法(RAFA)。     

壳聚糖—丝心蛋白合金膜的研究（Ⅱ）：半互穿聚合物网络型膜对…

研究了壳聚糖－丝心蛋白半互穿透合物网络型膜对ｐＨ值和离子的敏感性，发现该膜在ｐＨ〈３．３时溶胀度剧烈增加；在ｐＨ＝２时，是否出现溶胀极大值与膜组分的含量及交联剂的含量有关；膜在不同ｐＨ值溶液中可交替溶胀和收缩，且这种溶胀－收缩行为重复可逆，同时，该膜在不同离子溶液中的溶胀度亦不同，在相同离子强度的溶液中，此膜在３价离了了中的溶胀度最大。     

比值导数波谱法分析食品中抗氧化剂

利用混合物的波谱除以干扰组分的波谱得比值波谱，对波长求导得比值导数波谱，由此可消除干扰组分的吸光度叠加效应。该法能有效地对三组分混合物体系进行分析。利用此法对没食子酸丙酯(PG)、2，4，5-三羟基丁酰苯(THBP)和叔丁基对苯二酚(TBHQ)所组成的三组分混合体系进行分析，结果满意。     

比值导数波谱法分析混合色素

本文叙述了比值导数波谱法的原理，该法以混合物的波谱除以干扰组分的标准波谱面得到比值波谱，以比值波谱对波长求导得到比值导数波谱，由此得到的波谱可完全消除干扰组分的吸光度贡献。采用此法能方便地对二组分混合体系进行分析，如选择合适的零交点，则可对二组分混合体系进行分析。利用此法对胭脂红、日落黄及柠檬黄三种色素的二组分及三组分混合体系进行了分析，均获较好的结果。     

主成分分析同时单点pH滴定法研究

本文将主成分分析用于多组分同时单点ｐＨ滴定法中,讨论了方法原理,指定ｐＨ值的选择,建立了主成分分析常数矩阵,对四组分醇酮氧化酸试样及模拟样进行了多次测定,均获得了满意结果。     

固定pH跨度法滴定弱酸（碱）混合体系

１引言为了克服固定ｐＨ法在酸、碱干扰组分存在时，无法扣除空白的问题，我们提出了固定ｐＨ跨度法。当溶液的温度、离子强度及滴定剂浓度不变，滴定极弱酸（碱）至ｐＨ为Ａ时，消耗滴定剂体积ＶＡ与极弱酸（碱）的含量。之间存在如下关系：当滴至ｐＨ为Ｂ时（设此时反应还未完全），（２）－（１）得：αＡ、αＢ只与极弱酸（碱）的性质和ｐＨ值有关。故对于某一极弱酸（碱），当ｐＨ跨度一定时，△α为一常数，可通过滴定纯品测得。由于只取不完全质子化（失质子化）反应时由某一固定ｐＨ跨度而无须先加入强酸（碱）使待测组分完全质子化…     

比值导数波谱法分析食品中混合色素

利用混合物的波谱除以干扰组分的波谱得比值波谱,对波长求导得比值导数波谱,由此可消除干扰组分的吸光度叠加效应。该法能有效地对三组分混合体系进行分析。利用此法对亮蓝、日落黄、胭脂及柠檬黄等色素所组成的二组分和三组分混合体系进行分析,取得满意效果。     

校正变换矩阵法及其在多组分直接同时测定中的应用

将目标变换因子分析中自由浮动技术引入多元校准中，提出了一种新的多组分同时校准法———校正变换矩阵法。该法用于四组分氨基酸人工混合样品分析，结果令人满意，通过与传统目标变换因子分析法比较研究，表明该法用于组分光谱严重共线的波长范围时，其校准能力大大优于传统目标变换法。     

pH配位滴定法同时测定铜和锌

本文将多元线性回归法应用于ｐＨ配位滴定法中，提出了金属离子混合液中各组分同时测定的方法原理，并对铜，锌合成样品进行了测定，得到满意的结果。     

Simultaneous determination of oxygen and cadmium in cadmium and cadmium compounds

Cadmium and its compounds were analysed for oxygen and cadmium by a modification of the Schütze-Unterzaucher method. Oxygen in some compounds such as cadmium oxide, nitrate and sulphate could not be determined by the usual method. The method of adding carbon was employed for the determination of total oxygen. Total oxygen could be determined by the addition of 5 mg of carbon to a sample boat and heating at 950 degrees . The determination was also carried out by addition of naphthalene (2 mg). It was found that the cadmium powder and cadmium flake used contained ca. 1 and 0.15% oxygen, respectively. Oxygen and cadmium in cadmium and its compounds were simultaneously determined by the addition of 2 mg of naphthalene. Cadmium was determined colorimetrically by use of glyoxal-bis-(2-hydroxyanil). Oxygen and cadmium in the samples could be determined simultaneously with an average error of -0.02 and -0.22%, respectively.     

High-throughput synthesis and analysis of acylated cyanohydrins

The yields and optical purities of products obtained from chiral Lewis acid/Lewis base-catalysed additions of alpha-ketonitriles to prochiral aldehydes could be accurately determined by an enzymatic method. The amount of remaining aldehyde was determined after its reduction to an alcohol, whilst the two product enantiomers were analysed after subsequent hydrolysis first by the (S)-selective Candida antarctica lipase B and then by the unselective pig liver esterase. The method could be used for analysis of products obtained from a number of aromatic aldehydes and aliphatic ketonitriles. Microreactor technology was successfully combined with high-throughput analysis for efficient catalyst optimization.     

共振瑞利散射法对普萘洛尔特效适配体系的手性分析

本文提出了对于手性药物普萘洛尔手性识别和手性分析的新方法。 该方法引用基于氧化石墨烯的指数富集配体系统进化筛选技术(GO-SELEX),经过10轮优化筛选出对心血管药物普萘洛尔有高度亲和力的特效适配体。 然后通过共振瑞利散射光谱法(RRS)对反应体系进行特效性检测,实验表明S-普萘洛尔和R-普萘洛尔有迥然不同的光谱差异,S-普萘洛尔与特效适配体结合后的RRS显著增强,而R-普萘洛尔与适配体结合后的RRS几乎没有变化。 据此可以对心血管药物手性普萘洛尔进行有效的手性识别。 在考察反应体系和实验条件的基础上,可对S-普萘洛尔进行实验检测,同时对外消旋体中的R-普萘洛尔进行计算分析。 实验对S-普萘洛尔的线性范围为5~275 nmol/L,检测限为0.5 nmol/L。 方法应用于外消旋药片的分析检测,结果令人满意。 实验表明,RRS检测特效适配体结合的手性靶标体系会彰显不同的光谱差异,从而可对手性对映体进行手性识别,尤其是可利用其光谱差异实现同时测定的手性分析,方法可在特殊情形下不经分离而同时测定手性对映体,具有推广应用价值。     

Characterization of mixtures of biocidal oligoguanidines by capillary electrophoresis and high-performance liquid chromatography coupled to mass spectrometry

The polycondensation of guanidine hydrochloride and 2,2′-(ethylenedioxy)bis(ethylamine) leads to various types of oligomeric guanidines exhibiting a broad spectrum of biocidal activities. In the present work a reversed-phase high-performance liquid chromatographic method with a gradient consisting of aqueous 0.1% trifluoroacetic acid and acetonitrile as mobile phase has been developed to separate these oligoguanidines according to type and chain length. The combination with electrospray mass spectrometry allowed the identification of the various compounds. By this technique, some structures already suggested in the literature could be confirmed, and several additional oligoguanidines not yet reported could be identified. As a complementary technique, capillary zone electrophoresis was investigated. Best results were obtained with carrier electrolytes consisting of phosphoric acid in water/acetonitrile mixtures. Although the number of peaks that could be separated by the electrophoretic method was considerably lower than in case of the chromatographic method, capillary electrophoresis in combination with UV detection at 195 nm may still be a fast method suitable for quantitation of some of the major compounds and for monitoring the reaction rate during the polycondensation reaction.     

A chelate-forming resin bearing mercapto and azo groups and its application to the recovery of mercury(II)

A new chelate-forming resin bearing mercapto and azo groups was prepared from a common anion-exchange resin by treatment with azothiopyrine disulphonic acid (ATPS). ATPS resin was very stable and highly effective for the collection of mercury(II) by the batch and column methods. In the column method, the amount of mercury(II) in solution could be reduced to below 0.5 mug/l. The mercury(II) adsorbed could be eluted with thiourea solution, and the resin could be used repeatedly.     

An on-line galvanic cell-generated electrochemiluminescence and flow injection determination of calcium in milk and vegetables.

An on-line Ag/Al galvanic cell was studied and employed to generate electrochemiluminescence (ECL) of calcein blue. The potential of the galvanic cell could be adjusted by varying the components of flow reagent or by using different metals to substitute for Ag or Al. The reported cell exhibited perfect capability of supplying a stable potential for ECL generation. Because the weak ECL of calcein blue could be greatly sensitized in the presence of calcium in alkaline solution, calcium contents in milk and vegetable samples were assayed; the results were validated with ICP-AES method. The method gave linear results in 1.0 x 10(-4) mol L(-1) to 8.0 x 10(-6) mol L(-1) calcium concentration range and the 3(sigma)limit of detection was to be 2.0 x 10(-6) mol L(-1). Experiment results imply that this model of ECL detection could be applied for instrument miniaturization with easy fabrication.     

水凝胶微流控芯片的快速加工及在细胞培养检测中的应用

采用具有紫外光聚合性能的聚乙二醇(PEG)基水凝胶材料, 通过紫外光聚合作用快速加工双层水凝胶微流控芯片, 并验证了其对肿瘤细胞代谢液进行检测的可行性. 与传统微流控芯片材料相比, 该水凝胶芯片材料具有更好的生物相容性及可操控性, 可直接加工成形, 在生物学领域特别是细胞培养过程控制方面具有良好的应用前景. 实验结果表明, 该水凝胶微流控芯片可在微尺度空间有效模拟细胞生长环境, 并实现对细胞连续捕获后的原位培养. 将该芯片与卟啉可视阵列传感器系统结合, 经代谢特征分析可有效区分不同种类肿瘤细胞, 实现芯片细胞培养平台上的细胞代谢指纹快速可视化传感检测.     

HELP法在中草药分析中的应用研究-冬虫夏草的化学成分测定

基于直观推导式演进特征投影（ＨＥＬＰ）法,对冬虫夏草子座和虫体分别进行了多组分同时定性定量测定．结果表明,ＨＥＬＰ法能减少样本提取分离的步骤,降低色谱分离条件的要求,提高检测准确度．联用色谱检测与化学计量学解析法相结合将为复杂中草药分析提供一种全新手段     

Development and application of a biosensor for hypoxanthine in fish extract

A hypoxanthine biosensor was constructed using immobilized xanthine oxidase and a polarographic electrode. The enzyme was covalently immobilized on a commercially available preactivated nylon membrane. The polarographic electrode detected hydrogen peroxide and uric acid released during the enzymatic reaction. The electrode responded linearly to hypoxanthine concentration in the range 3.6–107 μM. When applied to the determination of hypoxanthine in several fish meats, the results obtained agreed well with those obtained by the conventional enzymatic method. More than 40 assays could be performed with the same membrane and each sample could be assayed in ca. 2–3 min. The biosensor provides a reliable, simple, rapid and economical method for the measurement of hypoxanthine, a useful indicator of fish freshness.     

Determination of phosphate in natural waters by capillary electrophoresis Influence of solution composition on migration time and response

This paper deals with the determination of the more complex phosphate anion by capillary electrophoresis using indirect UV detection. First, the pH of the running electrolyte influences both the migration time and the response of the phosphate anion. Both effects could be explained well by taking into account phosphorus speciation in solution. In addition, the experimental method has been applied to three different sets of natural water systems; (i) groundwater, (ii) surface water and (iii) stemflow samples. The migration time behaviour of phosphate was different for the three sample sets and, hence, difficulties arise with respect to a clear and unique identification of the compound. Deviations herein could be minimized by applying a correction method for migration time drift. Concentrations of phosphate could be quantified in most samples and were confirmed by a calorimetric method. Average recoveries of additions of phosphate to groundwater, surface water and stemflow samples were 105, 83 and 103%, respectively. For one stemflow sample, quantitative recovery of phosphate was possible only by changing the pH of the running electrolyte solution. The latter observation might be very useful in setting up speciation-related measurement methods.