四羧基铝酞菁与硫酸庆大霉素相互作用的共振散射光谱及其分析应用

在弱酸性介质中, 四羧基铝酞菁和硫酸庆大霉素本身的共振散射(RLS)均较弱, 但两者相互作用形成离子缔合物时, RLS显著增强, 在350～500 nm之间有一个强散射带, 最大散射峰位于401 nm. 而且散射强度与硫酸庆大霉素的浓度成正比, 可用于硫酸庆大霉素的定量测定, 线性范围为0.025～1.5 μg/mL, 检出限0.018 μg/mL. 方法可用于市售硫酸庆大霉素注射液含量的测定.     

基于与铁氰化钾和Zn~(2+)作用共振光散射法测定异烟肼

在酸性介质中,异烟肼能将铁氰酸根离子还原成亚铁氰酸根离子,后者与硫酸锌反应生成K2Zn3[Fe(CN)6]2粒子引起体系的共振光散射信号显著增强.在345nm处增强的散射信号强度ΔIRLS与异烟肼的浓度在0.01~1.0μg/mL范围内呈线性关系,据此建立了一种检测异烟肼含量的共振光散射(RLS)分析方法.线性回归方程为ΔIRLS=136.1+4239c(c,μg/mL),相关系数(r)为0.9984,检测限(3σ)为3.8ng/mL.该方法已成功用于异烟肼片剂及血清样品的测定.此外,文中还结合吸收光谱,动态光散射,扫描电子显微镜等表征手段对反应机理和RLS信号强度增强的原因进行了探讨.     

丽春红G与妥布霉素的共振散射光谱研究及其分析应用

在弱酸性条件下,丽春红G和妥布霉素反应后形成的产物导致体系的共振散射强度急剧增强,并在276、382和597 nm波长处产生3个新的共振散射峰,最大散射波长为597 nm.研究了反应的适宜条件和体系的光谱特征,妥布霉素的浓度在0.05~6.88μg/mL范围内与共振散射强度(ΔIRS)呈良好的线性关系,线性回归方程为△I597 nm=1.52c-2.68(R=0.9986),方法的检出限(3σ)为22.9 ng/mL.方法已用于硫酸妥布霉素注射液和滴眼液中含量的测定,结果满意.     

锌-硫氰酸盐-结晶紫体系共振散射法测定痕量锌

在pH 5.0 NaAc-HAc介质和吐温80溶液中,研究了zn(SCN)42-与结晶紫形成的离子缔合微粒的共振散射光谱,考察了其各种影响因素和适宜的反应条件,确定了共振散射强度与Zn2+浓度的关系,建立了测定痕量zn(Ⅱ)的共振散射新方法.研究表明,在0.020～0.80μg/mL范围内,体系的共振散射强度△I与Zn...     

蛋白质-SDS-罗丹明B体系的共振光散射光谱及其分析应用

研究了阴离子表面活性剂十二烷基硫酸钠(SDS),阳离子染料罗丹明B,与蛋白质相互作用的共振光散射(RLS)光谱及用于蛋白质的测定.实验表明,在pH 4.35的酸性介质中,SDS的共振光散射强度较小,它与蛋白质结合后,共振光散射强度能得到增强,但加入阳离子染料罗丹明B后,共振光散射强度显著增强.在λ=332.0 nm处,ΔIRLS最大,并且增强的共振光散射信号与蛋白质的浓度成正比.据此建立了一种测定蛋白质的新方法,该方法灵敏度高,对HSA的检出限达到1.9 ng/mL,线性范围为0.01～5.0 μg/mL.用于人血清样品中蛋白质的测定,回收率为94.0%～105.5%.     

共振光散射法测定对乙酰氨基酚

在酸性介质中,对乙酰氨基酚将铁氰酸根离子还原成亚铁氰酸根离子,后者与硫酸锌反应生成K2Zn3[Fe(CN)6]2粒子引起体系的共振光散射信号显著增强,且波长345 nm处增强的散射信号强度△IRLS与对乙酰氨基酚的浓度在0.01～1.0 μg/mL范围内呈良好线性关系.其线性回归方程为△IRLS=-15.01+4214...     

花菁-脱氧核糖核酸的共振光散射光谱及其分析应用

研究了一种苯并噻唑阳离子花菁与脱氧核糖核酸(DNA)作用的共振光散射光谱,在pH 6.0的六次甲基四胺-HCl缓冲介质中,痕量DNA的加入使花菁在590nm的共振光散射强度显著增强。在最佳实验条件下,增强的共振光散射强度与DNA浓度具有良好的线性关系,据此建立了一种测定DNA的共振光散射光谱法。方法的线性范围为:小牛胸腺DNA(CT DNA),0～20μg/mL,鱼精子DNA(FS DNA),0～15μg/mL;检出限分别为0.005μg/mL和0.008μg/mL。该方法已用于合成样品中DNA的测定。     

苯唑西林与维多利亚蓝B的共振瑞利散射光谱及应用

在pH 9.54时,苯唑西林的水解产物与维多利亚蓝B形成紫红色的离子缔合物,使体系的共振瑞利散射(RRS)急剧增强并产生新的RRS光谱,在最大散射波长366 nm处,苯唑西林的浓度在0~6.0μg/mL范围内与散射强度(△IRRS)成良好的线性关系,据此建立了测定苯唑西林的共振瑞利散射法,检出限为0.039μg/mL。该方法可用于苯唑西林药物及人体尿液中苯唑西林含量的测定。     

溴代十六烷基吡啶光谱探针RRS法测定硫酸皮肤素

研究了溴代十六烷基吡啶与硫酸皮肤素发生缔合反应的条件、共振瑞利散射特征.结果表明,在pH5.0的BR缓冲溶液中,硫酸皮肤素能与溴代十六烷基吡啶形成离子缔合物,使共振瑞利散射RRS急剧增强并产生新的RRS光谱.硫酸皮肤素浓度在0.015μg/mL～2.5μg/mL之间与散射强度呈线性关系,方法具有较高的灵敏度,其检出限(3σ)为4.5ng/mL,还研究了共存物质的影响,表明该方法选择性较好.该法用于血样和尿样中硫酸皮肤素含量的测定,结果令人满意.     

AR-Ag(Ⅰ)体系的共振散射光谱法测定痕量银

在pH=4.4的NaAc-HAc缓冲介质和2.0×10-3mol/L十二烷基苯磺酸钠(SDBS)溶液中,Ag(Ⅰ)与茜素红(AR)可形成较稳定的离子缔合物微粒,其在324、360和500nm处分别产生3个较强的共振散射峰.在最佳实验条件下,浓度在0.022～2.160μg/mL之间的Ag(Ⅰ)与共振散射强度△I324nm呈较好的线性关系,检测限为0.139 ng/mL.据此,建立了一种测定痕量银的共振散射新方法,并将该方法用于废胶片中痕量银的测定.     

同多酸和染料探针共振光散射法测定蛋白质

在酸性条件下,铬黑T、钼酸铵与蛋白质形成聚合物,使体系的共振光散射明显增强。据此建立了利用共振光散射技术测定总蛋白含量的新方法。在最佳条件下,体系的最大散射峰位于555nm处。共振光散射增强的程度与蛋白质的浓度呈良好的线性关系。牛血清白蛋白和人血清白蛋白的线性范围分别为0.20～10.0μg/mL和0.10～8.0μg/mL,检出限为0.050μg/mL和0.039μg/mL。方法已用于人血清样品的分析,并与考马斯亮蓝的测定结果进行了比较,两者无显著性差异。     

Study on naringenin-CTMAB-DNA system by resonance light scattering technique and its analytical application

A new high-sensitivity determination method of deoxyribonucleic acid (DNA) with detection limit at nanogram levels was proposed. Based on the measurement of resonance light scattering (RLS), it was found DNA could combine with naringenin and cetyltrimethylammonium bromide (CTMAB) in basic Tris-HCl buffer and produce enhanced RLS signal. The optimum conditions for this system were studied in detail. The enhanced intensity of RLS of naringenin-CTMAB at 353 nm was directly proportional to the concentration of DNA in the range of 0.017-1.7 μg mL(-1). The detection limit was 5.06 ng mL(-1). Using the proposed method, the synthetic samples were analyzed with satisfactory results, the recovery was 99.3-105.0% and RSD was 0.7-3.7%.     

A novel method for quantitative determination of tea polysaccharide by resonance light scattering

A new method for the determination of tea polysaccharide (TPS) in green tea (Camellia sinensis) leaves has been developed. The method was based on the enhancement of resonance light scattering (RLS) of TPS in the presence of cetylpyridinium chloride (CPC)-NaOH system. Under the optimum conditions, the RLS intensity of CPC was greatly enhanced by adding TPS. The maximum peak of the enhanced RLS spectra was located at 484.02 nm. The enhanced RLS intensity was proportional to the concentration of TPS in the range of 2.0-20 μg/ml. It showed that the new method and phenol-sulfuric acid method give some equivalent results by measuring the standard compounds. The recoveries of the two methods were 96.39-103.7% (novel method) and 100.15-103.65% (phenol-sulfuric acid method), respectively. However, it showed that the two methods were different to some extent. The new method offered a limit of detection (LOD) of 0.047 μg/ml, whereas the phenol-sulfuric acid method gives a LOD of 1.54 μg/ml. Interfered experiment demonstrated that the new method had highly selectivity, and was more suitable for the determination of TPS than phenol-sulfuric method. Stability test showed that new method had good stability. Moreover, the proposed method owns the advantages of easy operation, rapidity and practicability, which suggested that the proposed method could be satisfactorily applied to the determination of TPS in green tea.     

铁-金橙G-共振散射光谱法测定水中痕量Fe3+

研究了Fe3+-金橙G(OG)体系的共振光散射光谱,发现Fe3+对OG的共振光散射有增强效应。进一步研究发现,其增强值(△I)与加入Fe3+的质量浓度呈线性关系,对条件进行了优化,并建立了一种测定Fe3+的新方法,方法的线性范围为0.028～1.00μg/mL,检出限为0.009μg/mL,用于水样中痕量Fe3+的测定,结果满意。     

灿烂甲酚蓝共振光谱散射法测定脱氧核糖核酸

研究了灿烂甲酚蓝与脱氧核糖核酸（DNA）作用的共振光散射光谱,在pH＝10．8－11．5的范围内,DNA的加入导致灿烂甲酚蓝共振光散射的增强,在347nm处,存在一共振光散射增强峰,其强度与DNA的浓度呈线性关系,据此建立了一种测定DNA的共振光谱散射法。该方法的线范围为80－100μg/L,检出限为23．3μg/L.     

盐酸氯丙嗪作探针共振瑞利散射法测定环境水样中某些阴离子表面活性剂

在pH 3.0～5.0的HAc-NaAc缓冲溶液中, 盐酸氯丙嗪与十二烷基苯磺酸钠(SDBS)、十二烷基硫酸钠(SDS)和十二烷基磺酸钠(SLS)等阴离子表面活性剂反应形成离子缔合物时, 能导致共振瑞利散射(RRS)的显著增强并产生新的RRS光谱, 最大RRS峰分别位于277, 369和277 nm处, 方法对SDBS, SDS和SLS的检出限分别为0.018, 0.046和0.200 μg/mL, 其线性范围分别为0.09~10.0, 0.15~15.0 和0.67~12.5 μg/mL. 研究了适宜的反应条件及分析化学性质, 提出了一种用RRS技术灵敏、简便并快速测定阴离子表面活性剂的新方法.     

A Novel Protein Assay With an Azo Dye Using Rayleigh Light Scattering Technioque

ABSTRACT

The interaction of SPADNS [3-(4-sulfophenylazo)-4, 5-dihydroxy-2, 7-naphthalene disulfonic acid] with proteins in acidic solution was studied by spectrophotometric and Rayleigh light scattering (RLS) methods. SPADNS reacts rapidly with albumin at room temperature, and the intensity of the weak RLS of SPADNS was enhanced remarkably and quantitatively by this reaction.

Based on this observation, a novel RLS method for serum albumin determination was developed. The linear range is 0.125-14.9 μg/ml for BSA. The relative standard deviation (n=10) for 5.0 μg/ml BSA was 3.94%. The method was applied to the determination of proteins in human plasma, and the results were compared with the traditional proteins assay (CBB method). There is almost no interference from amino acids, metal ions and other coexistent substances. The reaction mechanism was also discussed.