流动注射氢化物发生电加热石英管原子吸收光谱法测血清硒

采用自控电热消化器消化血清 ,消化液经流动注射氢化物发生 电加热石英管 原子吸收光谱法测定血清硒。该方法的检出限为 0 .4 5ng·ml- 1,同一血样 8次测定相对标准偏差为 3 59% ,用该法测定了冻干牛血清标准物质和牛血清标准物质 ,测定结果均落在标准物质的不确定度范围内。方法准确、简便、灵敏 ,已用于临床血清硒样本的测定     

AGGREGATION CHARACTERISTICS OF LASER DYE RHODAMINE 6G IN AQUEOUS SURFACTANT SOLUTIONS

Abstract— –The role of surfactants as deaggregating agents for the laser dyes is investigated by spectrophotometry using Rhodamine 6G as a representative. A method to estimate the fraction of dye present as monomer, dimer and as a monomer-surfactant (monomer or micelle) complex is described. It is shown that among the surfactants, cetyl trimethyl ammonium bromide, Triton X-100, sodium lauryl sulfate (SLS) and potassium oleate, the anionic ones are the most effective in suppressing the aggregation of Rhodamine 6G. While the non-ionic surfactant is found to be effective only above its critical micellar concentration, the cationic surfactant has no effect on aggregation. The optimum concentration of SLS needed for suppression of dye-dimers is estimated.     

芦丁对罗丹明6G的荧光猝灭机理研究及其含量测定

根据Stem - Volmer方程和罗丹明6G吸收光谱的变化研究了芦丁对其荧光猝灭的类型及机理,结果表明,芦丁与罗丹明6G作用,形成一种稳定的复合物,而发生荧光静态猝灭,求得复合物的结合常数K=5.55×105L/mol,结合点数n=1.26.芦丁含量在0.92～137.8μg/mL范围内与F0/F成正比,检出限为0....     

DELAYED EMISSION OF CHLOROPHYLL a AGGREGATES AND RHODAMINE 6G EMBEDDED IN POLYMER MATRIX*

Delayed luminescence (in the microsecond time range) of the chlorophyll (Chl) a“dry” form as well as hydrated dimers located in a polyvinylalcohol film was measured from room temperature down to 8 K. In the same matrix the delayed luminescence of rhodamine 6G (Rhod) was investigated. The delayed emission both of Chl a and Rhod is probably due to the formation and delayed recombination of a radical pair. It seems that this process occurs without participation of triplet states, as it does not reflect their well-known sensitivity to oxygen. The temperature dependence of the delayed luminescence of vanous Chl forms is different. In the region around 678 nm (dry monomer) delayed luminescence needs a thermal activation energy of about 0.03 eV, whereas at 740 nm (wet aggregates) delayed luminescence intensity increases linearly with decreasing temperature. Its assignment as a-type delayed luminescence from the low-lying triplet state can consistently be excluded from both the weak temperature dependence of the delayed fluorescence and its large intensity as compared to the prompt fluorescence. Delayed luminescence of Rhod is almost independent of temperature between 8 K and 300 K. The dependence of delayed luminescence intensity on exciting light intensity is linear at lower intensities and tends to saturation at higher. Therefore the delayed luminescence is not related to exciton annihilation. Positions and intensities of the Chl delayed luminescence bands show that it is not phosphorescence (β-type delayed luminescence). The aggregation of both Chl and Rhod molecules strongly influences delayed luminescence since it differs in several properties if excited in the monomer or in the aggregate absorption range. Every aggregational form of dye emits its characteristic delayed luminescence band.     

罗丹明6G褪色光度法测定微量溴酸根

研究了在盐酸介质中,溴酸根氧化罗丹明6G褪色的最佳条件。吸收波长λmax为525nm,表观摩尔吸光系数为3.9×105L·mol-1·cm-1。溴酸根在0～5.0μg/5ml范围内符合比耳定律。方法用干合成样和化学试剂中微量溴酸根的测定,结果满意。     

GC-MS测定人血清中酞酸酯类环境污染物

为了解酞酸酯类环境污染物在人血清中的含量水平。采用毛细管柱气相色谱-质谱联用法的选择离子检测(GC-MS-SIR)技术,结合有机溶剂提取,高速离心去蛋白和低温浓缩的方法测定103份健康人血清中酞酸二丁酯(di--nbutyl phthalate,DBP)和酞酸二异辛酯[di-(2-ethyl-hexyl)phthalate,DEHP]。测定结果提示酞酸酯类环境污染物已进入人血清,DBP约为7.10 mg.L-1,DEHP约为6.78 mg.L-1,大部分人体内已有一定的污染负荷。     

新型双发色团固体激光染料薄膜的光稳定性研究

利用UV-Vis吸收光谱仪和光化学反应器研究了新型双发色团固体激光染料薄膜的光降解动力学.研究结果表明:双发色团固体激光染料薄膜的光褪色反应遵循假一级动力学衰减.在PRNAM系列共聚物(N-烯丙基-若丹明1、N-[(2-丙烯酸基)乙基]-1,8-萘酰亚胺和甲基丙烯酸甲酯的共聚物)中萘酰亚胺基团通过聚合物碳链与若丹明基团的氮原子相连;而在PRNM系列共聚物(若丹明1的烯丙基酯、N-[(2-丙烯酸基)乙基]-1,8-萘酰亚胺和甲基丙烯酸甲酯的共聚物)中则是与若丹明基团的酯基相连.PRNAM系列共聚物的光稳定性优于PRNM和PRM(若丹明1的烯丙基酯和甲基丙烯酸甲酯的共聚物)系列的光稳定性.     

高效液相色谱-质谱联用法测定人体血液中脂肪酸含量

建立了一种用液相色谱-串联质谱(HPLC- MS)快速、准确地对人体血液中游离脂肪酸进行分离和定量的方法.该法使用Dole提取法,提取的样品直接进行分析,无需衍生化处理.该方法以氘代十六烷酸为内标物,采用液相色谱-质谱联用法测定了人血清中游离脂肪酸的含量,各脂肪酸线性方程的相关系数均大于0.99,方法的回收率为90.0...     

阴极溶出伏安法测定人体血清中的痕量硒

用溶出伏安法测定人体血清中痕量硒的工作尚未见报导。本文对用阴极溶出伏安法测定人体血清中痕量硒的可能性及影响测试的因素进行了探讨,提高了可供实用的测试方法。     

气相色谱法测定人体血液中乙醇含量的测量不确定度评定

对气相色谱法测定人体血液中乙醇含量的测量不确定度进行评定。人体血液中乙醇含量测量结果的测量不确定度主要来源于相对定量校正因子、检材量、检材中添加内标物叔丁醇的体积、检材中乙醇峰面积的平均值与添加内标物叔丁醇峰面积的平均值之比、无水乙醇的纯度及密度等参数引起的不确定度。当检材中乙醇的含量为0．915mg／mL时,扩展不确定度为O．030mg/mL(k=2)。     

血清中胆固醇的国际比对--CCQM-K6的IDMS法测量

介绍血清中胆固醇的同位素稀释质谱测定法,首次报道了国际物质量咨询委员会（CCQM）2000年组织的血清中胆固醇测定的关键比对－CCQM－K6的结果。     

PROTOPORPHYRIN-SENSITIZED PHOTODYNAMIC MODIFICATION OF PROTEINS IN ISOLATED HUMAN RED BLOOD CELL MEMBRANES

Abstract— The photodynamic action of protoporphyrin on red cell ghosts is reflected by extensive cross-linking of membrane proteins to very high molecular weight protein aggregates. This process was studied with sepharose gel chromatography and sodium dodecyl sulphate polyacrylamide gel electrophoresis.
Most sensitive to this photodynamic effect are spectrin and band 2. 1, 2. 2, 2.3 and 4.1. polypeptides, which are cross-linked after very brief illumination periods, with a concomitant loss of spectrin-associated ATPase activity. Band 6 protein, representing the monomeric form of glyceraldehyde-3-phosphate dehydrogenase, is also very sensitive to protoporphyrin-induced cross-linking. The enzymatic activity decreased even faster than the amount of band 6 polypeptides, suggesting that modification(s) of the enzyme other than cross-linking, possibly by rapid photooxidation of a thiol group, may be responsible for inactivation.
Extracted and purified spectrin was cross-linked with about the same velocity as membrane-bound spectrin, reinforcing our previously drawn conclusion that membrane lipids are not involved in the cross-linking reaction. Eluted band 6 polypeptides on the other hand exhibited a relatively fast photo-oxidative modification but a much slower cross-linking to dimers and tetramers. This suggests that the membrane structure, e.g. the spectrin matrix may play an essential role in the incorporation of membrane-bound band 6 polypeptides in the high molecular weight cross-linked complex.     

邻—甲酚酞络合酮吸光光度法连续测定血清中钙和镁

利用邻－甲酚酞络合剂为显色剂建立了连续测定血清钙和镁的吸光光度法,钙和镁与该显色剂在ＰＨ１１的碱性缓冲液中形成紫色络合物,于５７０ｎｍ波长处均表最大吸收,且曲线具有加和性。先测得钙镁吸光度之和,加入８－羟基喹啉以掩蔽镁离子的干扰后测得钙的吸光度,两者之差即为镁的吸光度。钙和镁的摩尔吸光系数分别为２．１４×１０＾４和１．５１×１０＾４,方法应用于血清样品中钙和镁的连续测定,结果令人满意。     

GC-FPD、GC-MS法分析血液样品中的毒鼠强

采用液-液提取方法及GC—FPD定量、GC—MS定性检测手段，对血液样品中毒鼠强的提取和检测方法进行了研究。时提取毒鼠强的溶剂类型、溶剂用量及质谱分析参数等因素进行了考察，建立了一种回收率高、重现性好、灵敏度佳、干扰少的毒鼠强分析方法。毒鼠强工作曲线的线性范围为0．01-0．2μg／μL，相关系数r=0．9999，空白血液的加标平均回收率为93．6％，测定结果的相对标准偏差为5．27％。该方法满足司法鉴定中生物样品的定性、定量检验要求。     

THE PHOTOREACTION OF A RHODAMINE 6G MONOLAYER ADSORBED ON QUARTZ STUDIED BY SURFACE SECOND HARMONIC GENERATION

Abstract— A monolayer of rhodamine 6G on quartz in air exhibited photochemistry upon laser irradiation in the first absorption band. The course of the reaction was followed in real time by the surface second harmonic generation method. It was observed that the photoproduct had an enhanced non-linear coefficient, relative to rhodamine 6G. Absorption spectra showed that this was not a result of a stronger resonance enhancement of the signal by the photoproduct. Consideration of the factors to which the surface second harmonic signal is sensitive suggested that the enhancement arose from an increased charge transfer character of the photoproduct's electronic transitions, and a reorientation of its transition dipole.     

罗丹明类染料在分析化学中的应用进展

综述了90年代以来,罗丹明类染料在吸光光度分析,荧光分析,动力学分析等方面的应用,利用罗丹明染料进行测定的物质达50多种,且灵敏度很高。     

流动注射光度法同时测定血清中NO3^—和NO2^—

采用流动注射分析技术、以分光光度计为检测器,建立了同时测定血清中ＮＯ３和ＮＯ２的方法。以α－萘胺－７－磺酸为显色剂,在５２０ｎｍ比色,测定流路中装有锌－镉还原柱,将ＮＯ３在线还原为ＮＯ２。分析速度达４５样·ｈ＾－１,ＮＯ３和ＮＯ２的检出限分别为０．０１ｍｇ·Ｌ＾－１、０．００３ｍｇ·Ｌ＾－１,相对标准偏差分别为１．０％、０．５％。     

人血清蛋白的共振散射光谱法测定

在pH 7.0的缓冲介质中,吖啶黄(AO)与人血清蛋白(HSA)通过静电引力生成离子缔合物。与单独吖啶黄在相同溶液条件下相比,其共振散射光谱的强度有显著增强。在362 nm波长下所测得共振散射光谱峰的强度值与HSA的浓度值在0~1.3 mg.L-1范围内呈线性关系,并求得其检出限为32μg.L-1。上述反应条件已用于试样中HSA的测定。