双波长共振瑞利散射法测定皮蛋中的汞

建立了测定皮蛋中Hg的双波长共振瑞利散射新方法,研究了共振瑞利散射的光谱特征、共存物质的影响及反应机理。在pH 6.58的Tris-HCl缓冲介质中,Hg(Ⅱ)与快绿-溴代十六烷基吡啶结合生成三元络合物,使体系的双波长-共振瑞利散射(DWO-RRS)光谱显著增强,最大和次大的共振瑞利散射峰分别位于344 nm和470 nm波长处。当用双波长-共振瑞利散射(DWO-RRS)法测定时,Hg(Ⅱ)的质量浓度在0.005~0.50 mg/L范围内与体系的共振瑞利散射增强强度△I_(RRS)呈线性关系,检出限(3σ/S)为1.4 ng/mL,定量限为0.034 mg/kg。方法用于皮蛋中Hg的测定,回收率为98.2%~102%,相对标准偏差(n=5)为2.1%~2.7%。     

甲基蓝探针瑞利光散射测定奶制品中Cu(Ⅱ)

建立了检测奶制品中Cu(Ⅱ)的瑞利散射(RLS)法,探讨了适宜反应条件、反应机理、共存物质的影响及RLS光谱特征。在pH=5.50的Tris-HCl缓冲介质中,溴化十六烷基三甲基铵(CTMAB)增敏甲基蓝(MEB)使RLS信号显著增强,而Cu(Ⅱ)的加入则使体系的瑞利散射猝灭。在最大瑞利散射峰348nm处,Cu(Ⅱ)的质量浓度在0.007~0.13mg/L范围内与体系的RLS猝灭程度呈线性关系,检出限为0.0058mg/L,定量限为0.069mg/100g。方法用于奶制品中Cu(Ⅱ)的测定,加标回收率为98.4%~103%,相对标准偏差(RSD,n=6)为2.2%~2.8%。     

共振瑞利散射法测定药物及生物样品中的奥扎格雷钠

建立了快速测定药物及生物样品中奥扎格雷钠的共振瑞利散射(RRS)法。在弱碱性Tris-盐酸缓冲介质中,奥扎格雷钠与维多利亚蓝B反应生成离子缔合物,使共振瑞利散射信号显著增强,最大共振瑞利散射峰位于355 nm,在此处,奥扎格雷钠的质量浓度在0.002~0.4 mg/L范围内与共振瑞利散射增强程度△I_(RRS)呈线性关系,检出限为0.0018 mg/L。方法用于市售奥扎格雷钠药物、血液及尿样中奥扎格雷钠的测定,加标回收率为98.0%~102%,相对标准偏差为1.3%~1.8%。     

三元缔合物以双波长共振瑞利散射测定药物中酒石酸美托洛尔

建立了一种快速、准确测定药物中酒石酸美托洛尔的双波长共振瑞利散射(DWORRS)新方法。在酸性Tris-盐酸介质中,刚果红与酒石酸美托洛尔及表面活性剂十六烷基三甲基溴化铵反应生成红色三元缔合物,使双波长共振瑞利散射显著增强并产生新的具有2个明显散射峰的共振瑞利散射(RRS)光谱,最大共振瑞利散射峰位于375 nm,另一共振瑞利散射峰位于515 nm,酒石酸美托洛尔在0.004~0.55 mg/L范围内与体系的RRS增强强度的绝对值(│△I_(RRS)│)呈线性关系,检出限为0.0032 mg/L(375 nm),0.0038 mg/L(515 nm)和0.0018 mg/L(DWO-RRS,375 nm+515 nm)。还探讨了RRS的光谱特征、适宜反应条件、反应机理及共存物质的影响。方法用于药物中酒石酸美托洛尔含量的测定,加标回收率为98.57%~102.1%,相对标准偏差为2.0%~2.5%。     

橙黄Ⅳ探针共振瑞利散射光谱法测定大观霉素

建立了测定痕量大观霉素的共振瑞利散射(RRS)法。在弱碱性Tris-HCl缓冲介质中,大观霉素与橙黄Ⅳ相互作用后,共振瑞利散射显著增强,在352nm处的△IRRS最强。大观霉素的质量浓度在0.6~4.0mg/L范围内与△IRRS成正比,检出限(3Sb/S)为0.084mg/L。该法可用于市售大观霉素药物及人尿中大观霉素含量的测定,回收率为98.6%~101.5%。     

高灵敏共振瑞利散射法测定药物中的乌拉地尔

建立了一种快速测定药物中乌拉地尔的高灵敏共振瑞利散射(RRS)法,研究了RRS的光谱特征、反应条件及共存物质的影响。在p H 3.38的Tris-盐酸介质中,乌拉地尔与溴代十六烷基吡啶-偶氮氯膦Ⅲ反应生成三元离子缔合物,导致共振瑞利散射显著增强并产生新的RRS光谱。在最大共振瑞利散射峰374 nm波长处,乌拉地尔在0.002~0.37 mg/L范围内与缔合物的RRS增强强度的绝对值(│△IRRS│)呈线性关系,检出限为0.0016 mg/L。该法用于药物中乌拉地尔含量的测定,加标回收率为99.0%~99.7%,相对标准偏差(n=5)为1.6%~2.0%。     

溴代十六烷基吡啶增敏共振瑞利散射法测定药物中的维生素B_1含量

在pH 6.38的三羟甲基氨基甲烷-盐酸缓冲溶液和溴代十六烷基吡啶存在下,维生素B_1与氯酚红结合生成的缔合物使共振瑞利散射显著增强并产生新的共振瑞利散射光谱,最大共振瑞利散射峰位于339nm处,维生素B_1的质量浓度在0.03~0.42mg·L~(-1)内与其对应的共振瑞利散射增强程度(ΔI/_(RRS))呈线性关系,检出限(3s/k)为0.004 2mg·L~(-1)。据此提出了溴代十六烷基吡啶增敏共振瑞利散射法测定药物中的维生素B_1的方法。应用此方法分析了维生素B_1药物,加标回收率在99.2%~102%之间,测定值的相对标准偏差(n=6)在2.1%~2.5%之间。     

盐酸吖啶黄-脱氧核糖核酸反应体系的共振瑞利散射及其应用

研究了盐酸吖啶黄与脱氧核糖核酸(DNA)之间的共振瑞利散射(RRS)增强作用,提出了共振瑞利散射技术测定核酸的方法。在pH 6.4的B-R缓冲溶液中,盐酸吖啶黄与脱氧核糖核酸结合使溶液共振瑞利散射强度增强,其最大散射峰位于505 nm处,而在330 nm波长处有一稍弱的散射峰。DNA质量浓度在0.04~0.80 mg.L-1范围内,与RRS强度呈线性关系,检出限(3S/N)为0.023 mg.L-1。应用于测定合成样品中DNA含量并测得回收率为98.0%~104.0%。初步探讨了反应机理,盐酸吖啶黄与DNA间的相互作用包含有静电引力、π-π堆积力。     

铬天青S瑞利光散射技术快速测定面制食品中的Al

研究了在酸性Tris-盐酸缓冲介质和表面活性剂溴化十六烷基三甲基铵存在下,Al(Ⅲ)与铬天青S反应的瑞利散射光谱,建立了定量测定Al(Ⅲ)的瑞利散射新方法。实验表明,体系的结合物使瑞利光散射(RLS)显著增强,并产生新的瑞利散射光谱。最大瑞利散射峰位于371 nm处,瑞利散射增强程度(ΔIRLS)与0.016~0.54 mg·L-1范围的Al(Ⅲ)的质量浓度呈良好的线性关系,方法的检出限为0.0035 mg·L-1。方法用于面制食品中Al的测定,回收率为98.1%~102%,相对标准偏差(n=6)为0.8%~1.3%。     

瑞利光散射技术快速测定鲜苹果中的苹果酸

在碱性Tris-HCl缓冲介质中,苹果酸与维多利亚蓝B反应生成蓝色二元离子缔合物,使瑞利光散射明显增强,在368nm波长处,瑞利散射增强程度(ΔIRLS)与苹果酸的质量浓度在0.002~0.27mg/L范围内呈线性关系,检出限为0.0018mg/L。实验探讨了适宜的反应条件及主要分析化学性质。该方法简便、快速,用于市售鲜苹果中苹果酸含量的测定,回收率为98.4%~101%,相对标准偏差(RSD,n=5)为1.8%~2.2%。     

瑞利光散射技术用于药物中盐酸米多君的测定

建立快速、准确、灵敏的检测药物中盐酸米多君的瑞利光散射(RLS)新方法。在pH 4.55 Tris-盐酸溶液和十六烷基溴化吡啶鎓溶液中,盐酸米多君与坚绿FCF 反应生成三元离子缔合物,使体系的RLS信号显著增强并产生具有2 个强散射峰的新RLS 光谱。在最大RLS 峰364 nm 处,盐酸米多君的质量浓度在0.004~0.35 mg·L^-1范围内与缔合物的RLS 增强强度(ΔIRLS)呈线性关系,检出限(3Sb/S)为0.0031 mg·L^-1。加标回收率和相对标准偏差(RSD)(n=5)分别为98.3%~102% 和1.0%~1.3%。该法用于药物中盐酸米多君含量的测定,结果满意。     

Fe_3O_4@ILs-β-CDCP磁固相萃取-电感耦合等离子体发射光谱法同时测定环境水样中铅和锑

本文制备了磁性固相萃取材料Fe_3O_4@ILs-β-CDCP,并对其进行了表征。详细考察了Fe_3O_4@ILs-β-CDCP萃取Pb(Ⅱ)和Sb(Ⅲ)的各种影响因素,如溶液pH值、样品体积、洗脱剂浓度和用量、洗脱剂类型、共存离子影响等。基于此,建立了磁固相萃取-电感耦合等离子体发射光谱法(ICP-OES)同时测定Pb(Ⅱ)和Sb(Ⅲ)的新方法。在优化的条件下,该方法对Pb(Ⅱ)和Sb(Ⅲ)的检出限分别为1.50和0.54ng/mL,相对标准偏差(RSDs)分别为5.9%和2.4%(n=6,c=100.0ng/mL)。将该方法应用于实际水样中Pb(Ⅱ)和Sb(Ⅲ)的测定,其回收率分别为77.8%~106%和82.4%~107%。方法具有检出限低、操作简便等优势。     

Flow injection analysis: Rayleigh light scattering technique for total protein determination

A novel flow injection analysis (FIA) method with Rayleigh light scattering (RLS) detection was developed for the determination of total protein concentrations. This method is based on the weak intensity of RLS of bromothymol blue (BB) (3',3"-dibromothymolsulfonephthalein) which can be enhanced by the addition of protein in weakly acidic solution. A common spectrofluorimeter was used as a detector. It was proved that the application of this method to quantify the total proteins in real samples by using bovine serum albumin was possible. The RLS signal was detected at lambda(ex)= lambda(em)=572 nm. The linear range was 7.0-70.0 microg mL(-1), the detection limit was 3.75 microg mL(-1), the reproducibility was 5.5% (n=7), and the sample throughput was 26 h(-1).     

Determination of Proteins at Nanogram Levels by Enhanced Rayleigh Light Scattering Technique with Tetra-Substituted Sulphonated Aluminum Phthalocyanine

In recent years, Rayleigh light scattering has become a new tool for determining the content of biological molecules and studying the interaction mechanism of organic dyes with biological molecules^[1]. According to the macroscopic fluctuation theory, in a transparent isotropic medium, when the light scattering is caused by molecular particles 20-fold smaller than the wavelength of the incident beam, the Rayleigh scattering law is obeyed, namely I∝1/λ^4[2]. However, if the wavelength of the incident beam is close to that of the absorption band of the molecular particles which exist as aggregates, Rayleigh scattering will deviate from the law and enhanced RLS can be expected^[3]. Using this technique, a method for the determination of proteins in aqueous solution has been developed based on the enhancement effect of proteins on die Rayleigh light scattering (RLS) of organic dyes^[4].     

曙红Y的共振光散射与共振荧光

研究了曙红Y（EY）的共振散射光谱、荧光光谱和吸收光谱,讨论了共振光散射与共振荧光的区别与联系。在EY水溶液三维荧光等高线光谱图中,瑞利散射线与荧光等高线有部分相交。EY的共振散射峰（525nm）介于荧光激发峰（514nm）和发射峰（536nm）之间。由光偏振实验,测得EY共振散射光谱525nm处的偏振度P=0．20。上述实验结果证明,EY的共振散射峰主要是共振荧光。在改变pH的实验中发现,EY共振光散射增强是由于酸碱平衡的移动导致荧光型体的形成。由于自吸收的影响,共振散射光强度与EY浓度之间不是严格的线性关系。     

Determination of nucleic acids with tetra-(N-hexadecylpyridiniumyl) porphyrin sensitized by cetyltrimethylammonium bromide (CTMAB) using a Rayleigh light-scattering technique

Using a common spectrofluorometer to measure the intensity of Rayleigh light-scattering (RLS), a method for determination of nucleic acids has been developed. At pH 10.24 and ionic strength 0.01 mol l-1 (NaCl), the Rayleigh light-scattering of the tetra-(N-hexadecylpyridiniumyl) porphyrin (TC16PyP) is greatly enhanced by nucleic acids in the presence of cetyltrimethylammonium bromide (CTMAB), with the scattering peak located at 311.8 nm. The enhanced RLS intensity is in proportion to the concentration of calf thymus DNA (ctDNA) in the range 0.2-6.0 microg ml-1 and to that of fish sperm DNA (fsDNA) in the range 0.05-3.0microg ml-1. The limits of detection are 0.016 microg ml-1 for calf thymus DNA and 0.023 microg ml-1 for fish sperm DNA when the concentration of TPP was chosen 2.0 x 10(-6) mol l-1. Four synthetic samples were determined satisfactorily.     

基于与HTPB相互作用共振光散射法测定Hg2+

在酸性介质中,汞(Ⅱ)与过量溴离子反应生成四溴合汞(Ⅱ)阴离子,后者进一步与1-十六烷基三苯基溴化膦((1-Hexadecyl)triphenylphosphonium Bromide,HTPB)通过静电作用形成离子缔合体,引起体系的共振光散射信号显著增强,最大散射波长位于291.0 nm处,增强的散射信号强度与Hg2+浓度在0.04～1.5μmol/L范围内呈线性关系,检测限(3σ)为4.0 nmol/L.讨论了体系的最佳反应条件及外来物质的干扰,同时研究了体系的吸收光谱,并探讨了反应机理.建立的共振光散射法用于环境水样中Hg2+的测定,RSD≤4.42%.     

铜（Ⅱ)-氟喹诺酮类抗生素螯合物与虎红体系的吸收和共振瑞利散射光谱及其分析应用研究

在pH 4.2~4.8的B-R缓冲介质中,莫西沙星（MXFX)和加替沙星（GTF)等氟喹诺酮类抗生素（FLQs)能与铜（Ⅱ)形成螯合阳离子,进一步与虎红（Tf)阴离子通过静电引力和疏水作用形成FLQs∶Cu（Ⅱ)∶Tf为1∶1∶1的离子缔合物,体系反应导致共振瑞利散射（RRS)显著增强并出现新的RRS光谱。两种药物的反应产物具有相似的光谱特征,最大RRS峰位于373 nm处,并在590 nm处有1个较小的散射峰。在373 nm处一定浓度的抗生素与散射增强（ΔI)成正比,MXFX和GTF的线性范围分别为0.031~7.8 mg/L和0.029~9.0 mg/L。据此建立了测定氟喹诺酮类药物的新方法,方法用于胶囊和人尿液中FLQs的测定并取得满意结果。同时对反应机理及RRS增强原因进行了讨论。     

The Interaction between Propranolol and Gold Nanoparticles and its Analytical Application

The addition of propranolol induced the aggregation of gold nanoparticles, and increased Rayleigh light scattering (RLS) intensity greatly. The interaction between them was studied by RLS spectrum, UV-Vis spectrum and transmission electron microscopy (TEM). Based on these results, a novel method was proposed for propranolol assay. With the combination of solid phase microextraction (SPME), the proposed method was successfully applied to determine propranolol in urine.     

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.