免疫纳米金催化氯金酸与羟胺反应-共振散射光谱检测痕量青霉素G

小粒径的金和免疫金纳米粒子对氯金酸-盐酸羟胺这一反应具有较强的催化作用,其产物在580 nm处有一共振散射峰。以半抗原青霉素G为模型,用粒径为9 nm的金纳米微粒标记羊抗兔青霉素噻唑蛋白抗体制备了青霉素G的免疫纳米金共振散射光谱探针。在pH5.4的柠檬酸-磷酸氢二钠缓冲溶液中,青霉素G与金标兔抗青霉素发生特异性结合生成胶体金免疫复合物,离心分离。取适量金标羊抗兔青霉素的上层清液做催化剂,在pH3.36盐酸-柠檬酸钠缓冲溶液－40μg/mL氯金酸－21.6μg/mL的盐酸羟胺条件下,进行催化反应后金纳米粒径增大,在580nm共振散射强度处增强。随着青霉素G浓度c增大,上层清液中免疫金纳米微粒数量降低,I580nm值降低。其降低值△I580nm与c在0.15-225 ng/mL范围内成线性关系,其回归方程为△I580nm=0.28c+5.16,检出限为0. 05 ng/mL。该法用于牛奶中青霉素G的检测,结果较好。     

甲基蓝-铕为光散射探针测定美他环素的共振瑞利散射及共振非线性散射法研究

在pH=5.50的HAc-NaAc缓冲体系中,低浓度的甲基蓝(MB)-铕稀土配合物的光散射较弱,将微量的美他环素(MTC)加入后体系的共振瑞利散射(RRS)、二级散射(SOS)和倍频散射(FDS)均显著增强,且光散射信号与MTC浓度在一定范围内呈良好的线性关系,据此建立了灵敏的测定美他环素的共振瑞利散射和共振非线性散射分析法.实验以RRS法考查了甲基蓝-铕-美他环素体系形成三元离子缔合物的适宜条件、影响因素等,并初步探讨了其反应机制.     

银纳米微粒共振散射光谱法测定羟基自由基及其应用

以柠檬酸三钠做还原剂,采用微波高压法制备了银纳米微粒。用高速离心纯化除去过量的柠檬酸三钠获得了纯银纳米微粒。纯银纳米微粒的共振散射峰位于470nm处。在pH4.0的HAc-NaAc缓冲溶液中,Fenton反应产生的羟基自由基可氧化银纳米微粒生成银离子,导致470nm处的共振散射光强度降低。过氧化氢的浓度在0.27-7.56gmol／L范围内与银纳米微粒470nm处的共振散射强度降低值△I470nm呈良好的线性关系,回归方程为△I470nm=24.3C＋13.8,相关系数为0.9959,检出限为0.23μmol／L。该方法用于筛选羟基自由基的清除剂,获得了满意的结果。     

夜蓝共振瑞利散射法测定七叶皂苷钠

在pH值为4.5～5.5的BR缓冲溶液中,七叶皂苷钠(SA)阴离子与夜蓝(NB)阳离子反应,形成1:1的离子缔合物并引起共振瑞利光散射(RRS)急剧增强和产生新的RRS.最大散射波长位于416nm处,并且七叶皂苷钠质量浓度在0.025～20×10-6g/mL范周内与散射强度(ΔI)呈线性关系,用于七叶皂苷钠分析具有较高的灵敏度,检出限为7.5×10-9g/mL.研究了适宜的分析条件和影响因素,共存物质的影响研究表明,方法的选择性较好,可满足针剂、片剂及尿液中七叶皂苷钠的测定.     

基于与Ce3+相互作用共振光散射法测定三磷酸腺苷二钠

在Tris-HCl缓冲溶液中, 三磷酸腺苷二钠(ATP)与铈离子(Ce³⁺)相互作用产生很强的共振光散射(RLS)信号。实验表明,增强的散射信号与ATP的浓度在2.0~24 μmol/L范围内呈线性关系,据此建立了一种测定三磷酸腺苷的共振光散射法,检测限(S/N=3σ)为51.25 nmol/L。研究了共存物质的影响,用于临床三磷酸腺苷注射液的测定, RSD=2.29%。     

DNA对Ru(bpy)_2(dppx)~(2+)-SDS体系共振光散射的猝灭作用及其应用

研究了Ru(bpy)2(dppx)2+-SDS-DNA(bpy=2,2′-联吡啶,dppx=7,8-二甲基-吡啶并[3,2-a:2′,3′-c]吩嗪)体系的共振光散射光谱。结果表明,在阴离子表面活性剂十二烷基硫酸钠(SDS)预胶束聚集体存在下,Ru(bpy)2(dppx)2+-SDS体系具有很强的共振光散射,DNA的加入使其共振散射光猝灭。探讨了反应机理。基于DNA对Ru(bpy)2(dppx)2+-SDS体系共振光散射的猝灭作用,建立了共振光散射法测定DNA的新方法。在最佳实验条件下,体系在393nm处的共振光散射猝灭程度与DNA的浓度呈线性关系,线性范围为0.01～1.2mg/L,检出限为1.5μg/L。     

聚丙烯酸与核酸相互作用的共振光散射光谱研究及其分析应用

研究了聚丙烯酸(PAA)与脱氧核糖核酸(DNA)相互作用的共振光散射(RLS)光谱.实验结果表明,在pH=2.0的B-R缓冲溶液中,PAA与DNA自身的共振光散射峰均较弱,但当二者发生静电作用形成复合物后,体系的共振光散射峰增强,散射增强程度则各不相同,其相对散射强度的顺序是fsDNA＞ctDNA＞yRNA.在一定范围...     

二苯胺磺酸钠共振光散射法测定牛尿中白蛋白的研究

研究了以二苯胺磺酸钠为共振光散射探针测定牛尿中牛血清白蛋白的分析方法.该方法基于在pH=3.0的Britton-Robinson缓冲溶液中,牛血清白蛋白(BSA)与二苯胺磺酸钠结合后有强烈的共振光散射作用,在λ=469 nm处,共振光散射强度最大且光散射的强度与BSA的浓度成正比.方法简便、快速、灵敏度高,对BSA的检出限为0.18 mg/L,线性范围为0.20～16 mg/L,相关系数r=0.996.该法用于牛尿样品的分析测定,结果满意.     

Zn(Ⅱ)-硫氰酸盐-人血白蛋白体系共振Rayleigh光散射增强法对水环境Zn(Ⅱ)的测定

研究了Zn(SCN)2-4配合物与人血清白蛋白结合的散射光谱.结果发现,Zn(SCN)2-4的加入导致体系共振Rayleigh光散射增强;在一定条件下,600 nm处峰增强程度与Zn(Ⅱ)量成线性关系.据此建立了共振Rayleigh光散射增强法检测痕量Zn(Ⅱ)的新方法.方法线性范围0.005～1.0 mg/L,线性回归方程△IRRS=5.20 308.21 PZn(Ⅱ),相关系数r=0.999 6,检出限1.5μg/L,RSD为1.5%～3.3%,加标回收率为95%～103%.该方法结果与原子吸收法基本吻合.     

厚朴酚-结晶紫-十二烷基硫酸钠体系的共振光散射光谱研究及分析应用

在pH=3.5的柠檬酸钠-盐酸缓冲介质中,阳离子染料结晶紫(CV)对厚朴酚/和厚朴酚与十二烷基硫酸钠( SDS)的共振光散射光谱有协同增强作用.在优化的实验条件下,在共振光散射波长为333 nm处,体系的共振光散射增加值与厚朴酚及和厚朴酚在0.02～5.33 μg/mL范围内呈良好的线性关系,检出限为1.88×10-4...     

铁氰化钾高灵敏共振瑞利散射法测定青霉素类抗生素

在稀HCl介质中,K3[Fe(CN)6]与阿莫西林(AMO)、氨苄西林(AMP)、氯唑西林钠(CLO)、羧苄西林钠(CAR)和青霉素钠(BEN)等抗生素药物在加热条件下反应生成结合产物,会导致溶液的共振瑞利散射(RRS)强度急剧增强,并产生新的RRS光谱,5种反应产物的最大散射峰均位于330 nm附近。在一定的浓度范围内,不同的反应体系散射强度(∆I)与药物浓度成正比,反应具有很高的灵敏度,K3[Fe(CN)6]对5种药物的检出限分别在4.61至5.62 ng·mL-1之间。本文研究了RRS的光谱特征和适当的反应条件,并讨论了反应机理和散射增强的原因,还考察了共存物质的影响,表明方法具有较好的选择性,可用于胶囊、片剂和人血清及尿液中青霉素类药物的测定。     

Resonance Rayleigh scattering, second-order scattering and frequency doubling scattering methods for the indirect determination of penicillin antibiotics based on the formation of Fe3[Fe(CN)6]2 nanoparticles

Under the HCl solution and heating condition, penicillin antibiotics such as amoxicillin (AMO), ampicillin (AMP), sodium cloxacillin (CLO), sodium carbenicillin (CAR) and sodium benzylpenicillin (BEN) could react with Fe(III) to produce Fe(II) which further reacted with Fe(CN)₆³⁻ to form a Fe₃[Fe(CN)₆]₂ complex. By virtue of hydrophobic force and Van der Waals force, the complex aggregated to form Fe₃[Fe(CN)₆]₂ nanoparticles with an average diameter of 45 nm. This resulted in a significant enhancement of resonance Rayleigh scattering (RRS) and non-linear scattering such as second-order scattering (SOS) and frequency doubling scattering (FDS). The increments of scattering intensity (ΔI) were directly proportional to the concentrations of the antibiotics in a certain range. The detection limits for the five penicillin antibiotics were 2.9–6.1 ng ml⁻¹ for RRS method, 4.0–6.8 ng ml⁻¹ for SOS method and 7.4–16.2 ng ml⁻¹ for FDS method, respectively. Among them, the RRS method exhibited the highest sensitivity and the AMO system was more sensitive than other antibiotics systems. Based on the above researches, a new highly sensitive and simple method for the indirect determination of penicillin antibiotics has been developed. It can be applied to the determination of penicillin antibiotics in capsule, tablet, human serum and urine samples. In this work, the spectral characteristics of absorption, RRS, SOS and FDS spectra, the optimum conditions of the reaction and the influencing factors were investigated. In addition, the reaction mechanism was discussed.     

Spectrophotometric determination of some penicillins with ammonium vanadate

A spectrophotometric method for determining some penicillins has been developed. A known volume of the penicillin solution-in phosphate buffer of pH 6.8 is boiled with ammonium vanadate solution-in sulphuric acid medium-for 10 min and the absorbance of the colour formed is measured at 750 nm. The excess of vanadate can also be determined volumetrically. The method has been successfully applied for the determination of penicillin G sodium, phenoxymethyl penicillin, ampicillin sodium, phenethicillin potassium, cloxacillin sodium and methicillin sodium. The procedure is also used for analysing some pharmaceutical preparations of these drugs, e.g., injections. The results obtained are in agreement with those of the B P 1973 methods.     

十二烷基苯磺酸钠-硫酸耐而蓝体系的共振瑞利散射光谱及其分析应用

提出了共振瑞利散射法(RRS)测定十二烷基苯磺酸钠(SDBS)的新方法。在pH为1.98～3.29的B-R缓冲溶液中,硫酸耐而蓝与SDBS结合生成离子缔合物,使溶液共振瑞利散射(RRS)增强,其最大散射峰位于760 nm,另在533 nm、400 nm有两个较弱的散射峰。SDBS的浓度在0.04～1.6 mg/L范围内,与RRS强度有良好的线性关系,对SDBS的检出限(3σ)达0.018 mg/L。研究了适宜的反应条件和影响因素,表明该方法灵敏、稳定。用于环境水样中阴离子表面活性剂含量的测定,回收率为95.9%～106.7%。     

曙红Y共振光散射探针测定盐酸丙米嗪

在弱酸性介质中,盐酸丙米嗪与曙红Y依靠静电引力和疏水作用力形成离子缔合物,使曙红Y溶液的吸收光谱、荧光光谱和共振光散射光谱发生变化。其中以共振光散射法灵敏度最高。据此,建立了使用曙红Y作为共振光散射探针测定盐酸丙米嗪的新方法。研究了体系的吸收光谱、荧光光谱和共振光散射光谱特征。在最大散射峰364 nm处,测得盐酸丙米嗪的线性范围为0.025～2.5μg/mL,检测限为5.32 ng/mL,并将方法用于药物中盐酸丙米嗪含量的测定。     

Detection of Penicillin via Surface Plasmon Resonance Biosensor

A method of using Au colloid to capture the decomposed product of penicillin, penicillamine, on a surface plasmon resonance(SPR) biosensor for the quantitative determination of penicillin was developed. Based on the decomposition of penicillin to generate penicillamine and penilloaldehyde, a high sensitive biosensor for detecting penicillin was also developed. In our experiment, it was penicillamine rather than penicillin that has been measured. This is because penicillamine contains a functional group that makes it self-assembling on Au colloid to increase the molecular weight so as to improve the surface plasmon resonance signal. On a UV-Vis spectrophotometer, a high concentration of penicilliamine-Au complex was determined, indicating that penicillamine was already well combined with Au colloid. The method, using the combination of Au colloid with penicillamine, proved to detect penicillin.     

螯合微粒共振散射光谱分析测定痕量钴

研究了螯合微粒共振散射光谱的分析应用。结果表明,在pH为9．5的NH3-NH3Cl缓冲溶液中,Co（Ⅱ）与DDTC形成稳定的螯合物微粒体系,存在共振散射效应。在一定质量浓度范围内,Co（Ⅱ）的质量浓度与共振散射强度（IRS）呈较好的线性关系。其线性范围为0．012～1．44μg／mL,检出限为0．0012μg／mL,用于针剂维生素B12中钴的测定,方法简单、灵敏度高、重现性好,结果满意。     

Resonance Rayleigh Scattering Method for the Determination of Raloxifene with Evans Blue

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Determination of sodium hyaluronate with some basic bisphenylnaphthylmethane dyes by resonance Rayleigh scattering method

In an acetic acid-sodium acetate buffer solution ofpH 3.6-6.8,a compound complex was formed between sodium hyaluronate (abbreviated as SH)and some basic bisphenylnaphthylmethane dyes,leading to a great enhancement of the intensity of resonance Rayleigh scattering(RRS)and giving a new RRS spectrum,with its maximum scattering peak near 280 um.It was also found that the intensity of RRS was directly proportional to the concentration of SH near the range between 0 and 3.0 mg/L.Based on these facts,a sensitive method for the determination of SH has been established.The method had good selectivity,and has been used for the determination of total amounts of SH in samples with satisfactory results.For the NB-SH system,the detection limit of SH was down to 13.7 ng/mL.     

多菌灵与Pd（II）体系的共振瑞利散射光谱及分析应用

在pH=10.0的Britton-Robinson（BR）缓冲溶液中,多菌灵与Pd(Ⅱ)反应形成1∶1的六元螯合物,导致共振瑞利散射（RRS）、二级散射（SOS）和倍频散射（FDS）显著增强,并产生新的共振瑞利散射光谱,其最大RRS、SOS和FDS波长分别位于309、606和310 nm。 在一定范围内,3种散射增强（ΔIRRS、ΔISOS和ΔIFDS）均与多菌灵的浓度成正比,反应具有较高的灵敏度,对于多菌灵的检出限分别为7.1×10-9 g/mL（RRS）、7.4×10-9 g/mL（SOS）和10.7×10-9 g/mL（FDS）。 据此提出了测定多菌灵的光散射新方法。 以灵敏度最高的RRS法为例,测定了西芹和市售农药中多菌灵的含量,结果与标准方法一致。 文中还对反应机理和散射增强的原因进行了讨论。