CdTe量子点作探针共振瑞利散射法测定肝素钠

在水相中低温条件下制备了巯基乙胺稳定的CdTe量子点(CdTe QDs).基于肝素钠(Heparin)对巯基乙胺稳定的CdTe QDs共振瑞利散射(RRS)的增强作用,同时二级散射(SOS)和倍频散射(FDS)也相应增强,建立了一种快速、简便、定量测定肝素的新方法,同时讨论了最佳反应条件和影响因素,以RRS为例,在311 nm处,RRS的光谱强度与肝素钠的质量浓度c/(I-I_0)有良好的线性关系(r=0.999 1),线性范围13.5～1000 ng/mL,检出限(3σ)为4.04 ng/mL.可用于血样中肝素钠的测定.

Abstract：

Aqueous cysteamine-capped CdTe quantum dots(QDs) were prepared under low temperature.A simple and rapid quantitative method for heparin determination was proposed, based on the fact that hepa-tin can enhance CdTe QDs resonance Rayleigh scattering (RRS) and the intensities of second-order scatter-ing (SOS) and frequency-doubling scattering (FDS).Factors affecting RRS for detecting heparin with cys-teamine-capped CdTe QDs were studied.At 311 nm, the RRS calibration plot of C/(I-I_0) with concen-tration of heparin was linear in the range of 13.5-1 000 ng/mL with a correlation coefficient of 0.999.The limit of detection (30) was 4.04 ng/mL.     

硫化镉量子点-硫酸依替米星体系的共振瑞利散射和共振非线性散射光谱研究及其分析应用

在弱酸介质中,硫化镉量子点(CdS-QDs)与硫酸依替米星(ETM)在静电引力和疏水作用力下,形成粒径更大的聚集体,导致共振瑞利散射(RRS)、二级散射(SOS)和倍频散射(FDS)显著增强,其最大散射峰分别位于310 nm(RRS),568 nm(SOS),320 nm(FDS).在一定范围内ETM浓度与三种散射增强程度(△I)成正比,可用于ETM的测定,其中RRS的灵敏度最高,其检出限(3σ)为1.6 ng/mL.考察了共存离子的影响,表明方法有良好的选择性.据此发展了以CdS-QDs作探针,高灵敏、简便测定ETM的共振瑞利散射新方法,用于人血清和尿样中ETM的测定,平均回收率在94.5%～113.7%之间.

Abstract：

In a medium of pH = 5.6, CdS quantum dots could react with etimicin sulfate to form larger aggregates by virtue of electrostatic attraction and the hydrophobic force, which resulted in a great enhancement in resonance Rayleigh scattering (RRS) and resonance non-linear scattering such as second-order scattering (SOS) and frequency doubling scattering (FDS). The maximum scattering peaks were located at 310 nm for RRS, 568 nm for SOS and 320 nm for FDS. The enhancements of scattering intensity (△I) were directly proportional to the concentration of etimicin sulfate (ETM) within a certain range. Of the three methods, RRS had the highest sensitivity, its detection limit (3σ) being 1.6 ng/mL. An examination of the effects of coexisting substances showed that the method had good selectivity. Based on these results, a new method, highly sensitive and simple, was developed, which can be used to determinate ETM by CdS-QDs as a probe. The recovery for the determination of ETM in human serum and uric samples was in the range of 94. 5%-113.7%.     

高锰酸钾共振瑞利散射法测定磺胺二甲嘧啶

在0.2 mol/L H_2SO_4介质中,磺胺二甲嘧啶(SM_2)和KMnO_4在加热条件下发生氧化还原反应生成MnO_2微粒,导致共振瑞利散射(RRS)增强,并产生新的散射峰.其最大散射波长位于595 nm附近,散射强度在一定范围内与SM_2的浓度成正比,据此建立了测定SM_2的共振瑞利散射(RRS)新方法.本方法具有较高的灵敏度,检出限为8.6 ng/mL.实验优化了测定条件.考察了共存物质的影响,表明方法具有良好的选择性,用于片剂中SM_2的测定,结果满意.

Abstract：

In 0.20 mol/L H_2SO_4 medium, a redox reaction took place between sulfadimidine (SM_2) and po-tassium permanganate to form MnO_2 particles by heating.As a result, new spectra of resonance rayleigh scattering appeared and their intensities were enhanced greatly.The maximum peak of RRS was located at approximately 595 nm, and the scattering intensities were proportional to the concentration of SM_2.Based on these results, a new method for the determination of SM_2 was established.The detection limit (3σ) was 8.6 ng/mL.The effects of coexistent substances were tested, and the results demonstrated that this meth-od had good selectivity.It has been applied to the determination of SM_2 in tablets with satisfactory results.     

共振瑞利散射法测定水产品中孔雀石绿

在pH=4.4的HC1-NaAc缓冲介质中,孔雀石绿(MG)以及钨酸盐溶液自身的共振瑞利散射(RRS)均十分微弱.但是当MG染料阳离子与钨酸根(WO42-)形成离子缔合物时,RRS急剧增强,并出现新的RRS光谱,其RRS峰分别位于339 nm,451 nm和591 nm处.在最大散射波长339 nm处.孔雀石绿浓度在0.060～2.8 μg/mL范围与散射增强(ΔⅠ)呈良好线性关系,因此可用于痕量孔雀石绿的测定.方法灵敏度高,检出限为18.1 ng/mL.本法用于鱼肉中孔雀石绿残留量的测定,结果满意.

Abstract：

In an experiment reported in this paper, the resonance Rayleigh scattering (RRS) of malachite green (MG) or tungstate anion was very weak in pH 4.4 HC1-NaAc buffer medium, but when MG cation reacted with WO42- anion to form an ion association complex, its RRS dramatically increased and a new RRS spectrum appeared with the RRS peaks at 339 nm, 591 nm and 451 nm. The intensity of RRS (ΔⅠ)was directly proportional to the concentration of malachite green in the range of 0.06-2.78 μg/mL at the maximum scattering peak of 339 nm. The method was shown to be sensitive and the detection limit for MG was 18.1 ng/mL. Thus a new method for the determination of MG was developed. When applied to the determination of malachite green residues in the flesh of fish, this method gave satisfactory results similar to those of the HPLC method.     

乙基紫共振瑞利散射法测定碘酸钾

在磷酸介质中,碘酸钾与碘化钾反应生成I-^3配阴离子,它可进一步与乙基紫形成离子缔合物,此时不仅能引起吸收光谱的变化,而且能导致共振瑞利散射（RRS）的显著增强并产生新的RRS光谱,其最大散射波长位于319nm．在一定条件下,其散射强度△I与碘酸钾浓度成正比,其线性范围在2．33×10^-3～3．00μg·mL^-1之间,方法具有极高的灵敏度,对碘酸钾的检出限为0．70ng·mL^-1,也具有良好的选择性,可用于食盐中碘酸钾的直接测定。     

乙基紫共振瑞利散射法测定碘酸钾

在磷酸介质中,碘酸钾与碘化钾反应生成I3-配阴离子,它可进一步与乙基紫形成离子缔合物,此时不仅能引起吸收光谱的变化,而且能导致共振瑞利散射(RRS)的显著增强并产生新的RRS光谱,其最大散射波长位于319 nm.在一定条件下,其散射强度△I与碘酸钾浓度成正比,其线性范围在2.33×10-3～3.00 μg·mL-1之间,方法具有极高的灵敏度,对碘酸钾的检出限为0.70 ng·mL-1,也具有良好的选择性,可用于食盐中碘酸钾的直接测定.     

氯化钡共振瑞利散射法测定蜂蜜中硫酸链霉素残留

在0．05mol／LHCl和2．0mg／mL Triton X-100介质中,氯化钡与硫酸链霉素（STP）在加热条件下反应生成BaS04微粒,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,最大散射峰位于338nm附近．在0．01～4．0ug／mL浓度范围内,反应体系RRS强度与药物浓度成正比．反应具有较高的灵敏度,对STP的检出限（3a）为4．8ng／mL．研究了适宜的反应条件和影响因素,并考察了共存物质的影响,表明方法具有较好的选择性,可用于蜂蜜中STP残留的检测．     

牛血清白蛋白共振瑞利散射和共振非线性散射法测定硫酸软骨素

在pH=2.8～4.0的BR缓冲溶液中,硫酸软骨素(CS)由于磺酸基离解而成为带多个负电荷的大阴离子,而低于其等电点(pI=4.7)的牛血清白蛋白(BSA)则以带正电荷的大阳离子存在,两者之间可结合形成复合物.此时将引起共振瑞利散射(RRS)显著增强,并产生新的RRS光谱,其最大散射波长位于304 nm处.与此同时,它的二级散射(SOS)和倍频散射(FDS)也明显增强,且最大SOS和FDS分别位于471 nm和292 nm.散射增强的强度(△I_(RRS)、△I_(SOS)和△I_(FDS)与CS浓度在一定范围内成正比,可用于CS的定量测定.对于CS的检出限(3σ)分别为2.0 ng/mL(RRS),2.9 ng/mL(SOS)和13.2 ng/mL(FDS).研究了适宜的反应条件,考察了共存物质的影响,表明方法有较好的选择性,可用于市售滴眼液中硫酸软骨素含量的测定.

Abstract：

In a Britton-Robinson (BR) buffer solution of pH 2.8--4.0, chondroitin sulfate (CS), which carries negative charge by the ionization of sulfonie group, reacted with bovine serum albumin, which car-ries positive charge through electrostatic force and hydrophobic interaction, to form a complex, resulting in a significant enhancement of resonance Rayleigh scattering (RRS) and the appearance of a new RRS spectrum with the maximum wavelength at 304 nm.At the same time, the second-order scattering (SOS) and frequency-doubling scattering (FDS) were enhanced obviously with a peak at 471 nm and 392 nm, re-spectively.The intensity of scattering (△I_(RRS), △I_(SOS) and △I_(FDS)) was directly proportional to the concentra-tion of CS in a certain range.When used in CS determination, this method exhibited high sensitivity, with a detection limit of 2.0(RRS), 2.9(SOS) and 13.2(FDS) ng/mL.The optimum conditions for the reac-tion and the influencing factors were investigated.The interference of foreign substances was examined and this method showed a good selectivity.The method can be applied satisfactorily to the determination of CS in eye drops.     

氯化钡共振瑞利散射法测定蜂蜜中硫酸链霉素残留

在0.05 mol/L HCl和2.0 mg/mL Triton X-100介质中, 氯化钡与硫酸链霉素(STP)在加热条件下反应生成BaSO4微粒, 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, 最大散射峰位于338 nm附近. 在0.01～4.0 μg/mL浓度范围内, 反应体系RRS强度与药物浓度成正比. 反应具有较高的灵敏度, 对STP的检出限(3σ)为4.8 ng/mL. 研究了适宜的反应条件和影响因素, 并考察了共存物质的影响, 表明方法具有较好的选择性, 可用于蜂蜜中STP残留的检测.     

牛血清白蛋白共振瑞利散射和共振非线性散射法测定硫酸软骨素

在pH=2.8~4.0的BR缓冲溶液中,硫酸软骨素(CS)由于磺酸基离解而成为带多个负电荷的大阴离子,而低于其等电点(pI=4.7)的牛血清白蛋白(BSA)则以带正电荷的大阳离子存在,两者之间可结合形成复合物.此时将引起共振瑞利散射(RRS)显著增强,并产生新的RRS光谱,其最大散射波长位于304 nm处.与此同时,它的二级散射(SOS)和倍频散射(FDS)也明显增强,且最大SOS和FDS分别位于471 nm和292 nm.散射增强的强度(ΔIRRS、ΔISOS和ΔIFDS)与CS浓度在一定范围内成正比,可用于CS的定量测定.对于CS的检出限(3σ)分别为2.0 ng/mL(RRS),2.9 ng/mL(SOS)和13.2 ng/mL(FDS).研究了适宜的反应条件,考察了共存物质的影响,表明方法有较好的选择性,可用于市售滴眼液中硫酸软骨素含量的测定.     

同多钨酸根共振瑞利散射光谱法测定硫酸奎宁

在pH=2.2～3.4的HCl-NaAc弱酸性介质中,硫酸奎宁和同多钨酸根相结合生成离子缔合物,能引起共振瑞利散射的显著增强,且散射强度与硫酸奎宁的浓度在一定范围内成正比,检出限为7.7 ng/mL.考察了共存物质的影响,表明该方法具有较好的选择性.用于汤尼水(Tonic Water)中奎宁的测定,结果满意.并对离子缔合物的形成和RRS增强的原因进行了讨论.     

酸性磺酞类染料共振Rayleigh散射光谱法测定奈替米星

用共振Rayleigh散射(RRS)光谱研究了酸性磺酞类染料溴甲酚绿和溴酚蓝分别与奈替米星的相互作用.溴甲酚绿和溴酚蓝在酸性介质中分别与奈替米星相互作用,导致RRS光谱显著增强,最大的RRS峰分别位于606nm和572nm处,散射强度与奈替米星的质量浓度在一定的范围内成正比.此方法具有很高的灵敏度,对于奈替米星的检测限(3σ)分别为30ng/mL和10ng/mL,据此发展了一种测定奈替米星的新方法.