MALDI－TOF－MS法分析人血清白蛋白

用基质辅助激光解吸附飞行时间质谱（ＭＡＬＤＩ－ＴＯＦ－ＭＳ）法分析测定了人血清白蛋白。结果表明，全军血液制品研究中心应用Ｒｉｖａｎｏｌ和Ｃｏｈｎ＇ｓ两种方法分离提取的人血清白蛋白，其分子量与理论计算值相吻合，其纯度与市售标准人血清白蛋白相一致，用ＭＡＬＤＩ－ＴＯＦ－ＭＳ法分析鉴定人血清白蛋白，准确、简便和灵敏（仅需ＰＭ浓度样品），且重复性好，日内和日间差的变异系数均小于０．０３％，是ＳＤＳ－ＰＡＧＥ电泳法所无法比拟的。     

新型固液双重致孔球形离子交换剂的制备及其性能研究

以甲基丙烯酸缩水甘油酯为单体 ,采用固液联合致孔方式 ,通过一步悬浮聚合制备了一种新型双孔高分子球形载体 .经化学修饰后 ,得到含二乙胺羟丙基的阴离子交换剂 (介质A) .优化了制备条件 .并与用相同方法制备的但仅含有机溶剂致孔剂的介质B进行了比较 .介质A和B均具有较高的静态吸附容量和机械强度 .由于介质A内含有流动相可以对流通过的大孔 ,因此其动态吸附容量远高于介质B ,并且在较高的流速下表现出较好的色谱流动性能     

Spectrofluorimetric determination of guanethidine sulphate,guanfacine hydrochloride,guanoclor sulphate and guanoxan sulphate in tablets and biological fluids,using benzoin

A sensitive and rapid Spectrofluorimetric method for the determination of guanethidine sulphate, guanfacine hydrochloride, guanoclor sulphate and guanoxan sulphate in tablets and spiked human serum and urine samples is described. The method is based on the reaction of monosubstituted guanidino compounds in an aqueous potassium hydroxide solution with benzoin, in the presence of -mercaptoethanol and sodium sulphite. Highly fluorescent derivatives were obtained, with excitation and emission maximum wavelengths around 325 and 430 nm, respectively. In optimal reaction conditions, the linearity ranges were 0.04–0.28 g/ml, with relative standard deviations less than 2%. The method has been successfully applied to the determination of these drugs in tablets. The results are highly correlated with the B.P. method. Chloroform (or for guanoxan dichloromethane) was used to extract the drugs from serum and urine at basic pH, followed by the proposed fluorimetric method. The limit of detection is 0.02 g/ml for the selected drugs.     

儿童易疲劳与血清中微量元素含量的相关性研究

测定了1562名儿童(其中包括153名易疲劳儿童)血清中Zn、Fe、Cu、Ca、Mn和Pb的含量。研究发现,易疲劳儿血清Ca含量(84.4±12.5μg/mL)显著低于对照组儿童(88.5 4±13.4μg/mL),P<0.05;Fe含量(1.094±0.22μg/mL)显著高于对照组儿童(1.07 4±0.22μg/mL),P<0.05;Mn含量(0.040 4±0.035μg/mL)非常显著高于对照组儿童(0.035 4±0.013μg/mL),P<0.001。     

Characterization of Ultrathin Films of Cellulose Esters

The adsorption of cellulose acetate (CA), cellulose acetate propionate (CAP) and cellulose acetate butyrate (CAB) from solutions prepared in acetone onto silicon wafers led to ultrathin films, which were characterized by ellipsometry, atomic force microscopy (AFM) and contact angle measurements. The polysaccharides films were characterized in the air just after their formation and after annealing at temperatures higher than their glass transition temperature or melt temperature. The films thickness close to 2 nm and surface roughness did not vary significantly upon annealing. AFM images revealed the presence of small clumps dispersed on a homogeneous layer, which covered completely the Si wafers. Such topographic details were also observed after annealing. However, upon annealing the films surfaces changed from hydrophilic to hydrophobic, evidencing molecular re-orientation at the solid–air interface. The adhesion of bovine serum albumin (BSA) and lipase onto the cellulose esters films was quantified in order to evaluate the possibility of applying such films as selective support for biomolecules.     

血清蛋白-荧光素复合物单扫极谱波与应用

在0．08mol／L的HAc中，荧光素与牛血清白蛋白(BSA)或人血清白蛋白(HSA)相互作用形成复合物。复合物使荧光素在-0．58V(vs．SCE)处的还原峰电流增大，峰电流的增大值与加入的BSA或HSA的浓度在一定的范围内呈线性关系。BSA在2—24μg／mL范围内呈线性关系，检出限为1μg／mL；HSA在2—22μg／mL范围里呈线性关系，检出限为0．8μg／mL。应用该法测定了人血清蛋白样品，结果令人满意。     

LC Packing Materials for Pharmaceutical and Biomedical Analysis

 The author has prepared novel liquid chromatography (LC) packing materials for pharmaceutical and biomedical analysis. Those include LC packing materials for direct serum injection assays of drugs and their metabolites, LC packing materials for resolution of enantiomeric drugs, and uniformly sized molecularly imprinted polymers for drugs and their metabolites.     

刚果红与血清白蛋白相互作用的极谱分析

在pH4．7HAc-NaAc缓冲溶液中，刚果红与蛋白质(BSA或HSA)作用形成络合物，使刚果红-0．35V(vs SCE)的还原峰电流下降，峰电流的降低值同所加的BSA或HSA质量浓度在一定范围内呈线性关系；BSA和HSA的线性范围分别为0．5～12mg／L和0．5～11mg／L，检出限分别为0．25和0．20mg／L；运用该法测定了人血清白蛋白样品，结果令人满意。     

A comparison of double-focusing sector field ICP-MS, ICP-OES and octopole collision cell ICP-MS for the high-accuracy determination of calcium in human serum

Human serum is routinely measured for total calcium content in clinical studies. A definitive high-accuracy and low-uncertainty method is required for reference measurements to underpin medical diagnoses. This study presents a novel octopole collision cell ICP-MS, high-accuracy, methodology and comparison of that technique with double-focusing sector field ICP-MS and an ICP-OES method. Double-matched isotope dilution mass spectrometry (IDMS) was employed for ICP-MS techniques and an exact matching bracketing technique using scandium as an internal standard was used for ICP-OES analysis. Medium resolution mode was utilised for double-focusing sector field ICP-MS analysis to resolve the dominant interferences on the ⁴⁴Ca/⁴²Ca isotope pair. Hydrogen reaction gas was employed to chemically resolve a number of polyatomic interferences predominantly through charge transfer reactions in the octopole collision cell. Comparison data presented for NIST CRM 909b human serum analysis from all three techniques demonstrates highest accuracy (99.6%) and lowest uncertainty (1.1%) for octopole collision cell ICP-MS. Data from ICP-OES using a non-IDMS technique produces comparably accurate data and low-uncertainties. The much higher total expanded uncertainties for double-focusing sector field ICP-MS compared with octopole collision cell data are explained by lower precision on the measurement of the ⁴⁴Ca/⁴²Ca isotope ratio. Data for octopole collision cell ICP-MS submitted for an international blind trial comparison (CCQM K-14) demonstrated excellent agreement with the mean of all participants with a low expanded uncertainty.     

荧光法研究Ge-132对牛血清白蛋白Maillard反应的抑制作用

人体内氨基酸及蛋白质的非酶糖化反应(Maillard反应)与糖尿病及其并发症的关系已经引起广泛注意[1].有机锗化合物β-羧乙基锗倍半氧化物(Ge-132)具有预防糖尿病及调节糖代谢的作用[2].