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.     

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.     

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.     

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.     

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.     

钯(Ⅱ)-托拉塞米反应体系的共振瑞利散射和共振非线性散射光谱及其分析应用

在pH=4.0～7.0的Britton-Robinson(BR)缓冲溶液中,托拉塞米与Pd(Ⅱ)形成1:1的螯合物,此时将引起共振瑞利散射(RRS)、二级散射(SOS)和倍频散射(FDS)显著增强,其最大RRS,SOS和FDS波长分别位于340,586,349 nm附近,在一定范围内,3种散射增强与托拉塞米的浓度成正比,方法具有较高的灵敏度,对托拉塞米的检出限(3σ)在1.1～5.5 ng/mL之间.考察了适宜的反应条件及共存物质的影响,表明方法有良好的选择性.据此,提出了测定痕量托拉塞米的灵敏、简便和快速的新方法.     

CdTe量子点作探针共振瑞利散射法测定甲氨蝶呤、头孢曲松钠

以巯基乙胺为稳定剂,在水相中合成CdTe量子点,巯基乙胺自组装在量子点的表面形成带正电的聚合体,在pH为5.0～5.6的弱酸性条件下,带正电的CdTe量子点聚合体与带负电的甲氨蝶呤(Methotrexate MTX)、头孢曲松钠(Ceftriaxone CTRX)通过静电引力及疏水作用力结合形成粒径较大的聚合体,这种聚合体的形成导致共振瑞利散射(Resonance Rayleigh Scattering RRS)强度显著增大,同时二级散射(seconol-order scattering SOS)和倍频散射(frequency-doubling scattering FDS)也显著增强.在一定条件下,散射增强(△I)与甲氨蝶呤、头孢曲松钠的浓度成正比,其中RRS方法有较高的灵敏度,甲胺蝶呤和头孢曲松钠的线性范围分别为0.01～4.50 μg/mL,0.03～4.20 μg/mL,检出限(3σ)分别为3.06 ng/mL,8.90 ng/mL.这种方法灵敏、简便、快速,可用于血样中甲氨蝶呤、头孢曲松钠的痕量分析.     

钯(Ⅱ)-盐酸吗啉胍螯合物与卤代荧光素染料相互作用的超瑞利散射光谱及其分析应用研究

在pH=4.4～5.0的HAc-NaAc介质中,钯(Ⅱ)与盐酸吗啉胍(Abob)反应形成螯合阳离子,它能进一步与二溴荧光素(DBF)、曙红Y(EY),赤藓红(Ery)阴离子反应形成离子缔合物,引起超瑞利散射(HRS)显著增强.3个三元体系具有相似的光谱特征,最大HRS波长位于390 nm附近.在一定条件下超瑞利散射增强(△IHRS)与Abob的浓度成正比,其线性范围是0.029～3.0μg/mL(DBF),0.14～3.5μg/mL(EY)和0.23～1.9μg/mL(Ery),检出限分别为0.008 6μg/mL(DBF),0.043 μg/mL(EY)和0.069μg/mL(Ery).研究了HRS法的适宜反应条件和共存物质的影响,发展了高灵敏、简便快速测定Abob的新方法,可用于尿样中Abob的测定.

Abstract：

In an acidic medium with pH = 4.4-5.0, palladium (Ⅱ) chelated with moroxydine hydrochloride to form the cation [ Pd (Abob)]2+ , which reacted further with dibromofluorescein (DBF), eosin Y (EY)and erythrosin(Ery) to form ion-association complexes, respectively. As a result, the hyper Rayleigh scattering(HRS) intensities were enhanced greatly. The maximum HRS peak of the three systems was all located at approximately 390 nm. HRS intensity was proportional to the concentration of moroxydine hydrochloride (Abob) in the range of 0. 029-3.0 μg/mL for DBF, 0. 14-3.5 μg/mL for EY and 0.23-1.9 μg/mL for Ery, and their detection limit (3σ) was 0. 008 6, 0. 043 and 0. 069μg/mL, respectively. The optimum conditions of the reaction and the properties of analytical chemistry were investigated. Therefore, a new method for the determination of moroxydine hydrochloride(Abob) by HRS was developed. The method has high sensitivity and good selectivity and has been applied to the determination of Abob in uric samples with satisfactory results.     

Relative bioavailability of tribasic zinc sulfate for broilers fed a conventional corn-soybean meal diet

An experiment was carried out to investigate the relative bioavailability of tribasic zinc(Zn) sulfate relative to Zn sulfate for broilers fed a conventional corn-soybean meal diet. A total of 504 1-d-old Arbor Acres commercial male chicks were randomly assigned by body weight of birds to one of seven treatments involving a 2×3 factorial arrangement with three levels of added Zn(30, 60, or 90 mg of Zn kg–1) and two Zn sources(tribasic Zn sulfate and Zn sulfate) plus a control with no added Zn for an experimental phase of 14 d. Plasma Zn, tibia ash Zn, pancreas Zn, and pancreas metallothionein(MT) messenger RNA(m RNA) were analyzed at 6 or 14 d of age post-hatching. The results showed that plasma Zn, tibia ash Zn, pancreas Zn, and pancreas MT m RNA increased linearly(P0.002) as dietary Zn concentration increased at 6 or 14 d of age. The R2 for a linear model was greater on d 6 than on d 14 for the above 4 responsive criteria, and among these indices, the fitting of the tibia ash Zn concentration was the best(R2=0.99). Therefore, based on slope ratios from the multiple linear regressions of the above 4 indices of the birds at 6 d of age on daily intake of dietary Zn, the bioavailabilities of tribasic Zn sulfate relative to Zn sulfate(100%) were 95.6%(P=0.18), 83.5%(P=0.01), 87.9%(P=0.53), and 75.9%(P=0.38) for the tibia ash Zn, pancreas Zn, plasma Zn, and pancreas MT m RNA, respectively. The results indicated that generally, Zn from tribasic Zn sulfate was as available as Zn from Zn sulfate for broilers.     

Effect of a bacterial inoculum and additive on dry matter in situ degradability of sugarcane silage

The objective of this study was to evaluate the effect of adding a bacterial inoculum and a handmade additive to sugarcane silage(SCS) on the in situ digestibility of dry matter(DM). The treatments were: T1) sugarcane silage(SCS) and T2) sugarcane silage with 1% inoculum and 1% additive(SCS+). The bacterial inoculum consisted of 10.0% molasses, 1.0% yogurt, 5.0% chicken manure, 0.5% urea, and 83.0% water, and the additive was formulated with 1.0% urea, 0.1% ammonium sulfate, and 0.25% phosphorus. In situ dry matter digestibility(DMD) was determined using the nylon bag technique with four cows equipped with ruminal fistulas. Cows were fed with ensiled sugarcane supplemented with 1 kg of commercial concentrate. 5 g of ground sample for each sugarcane treatment were weighted in nylon bags and incubated for 4, 8, 12, 24, 48, and 72 h in a completely randomized design with six replicates. The DMD(%) was higher(P<0.05) for SCS+ for all incubation times when compared with SCS. There were no differences in ruminal p H between the treatments for all the incubation times. The data suggested that the sugarcane silage with bacterial inoculum and additive could be an alternative for providing forage for ruminants during the season of low growth and quality grass.     

双波长共振光散射比率法及其在槲皮素分析中的应用

以槲皮素(QT)与Al3+的相互作用为例,建立了基于单次扫描光谱获得共振光散射信号升降变化的一种全新双波长比率法Al3+在醋酸-醋酸钠缓冲溶液中形成的羟基配合物,随槲皮素加入,槲皮素将羟基配合物中的铝竞争下来形成槲皮素与铝的配合物,使得280 nm处的散射强度(IRLS280)降低,444 nm处的散射强度(IRLS444)增强.结果表明Log(IRLS 280/444nm)与槲皮素浓度在(2.5～25)×10-5 mol/L范围内呈线性关系,相关系数R=0 998 0,检测限为2.0×10-6mol/L.     

共振光散射技术在核酸分析应用中的研究进展

综述了不同种类的共振光散射探针在核酸定量分析中的应用，并对共振光散射探针与核酸的作用机理进行了探讨。     

蛋白质纳米铁共振光散射探针的研究

[目的]探索定量测定核酸和蛋白质等生物大分子的方法。[方法]采用Fe(OH)3纳米粒子作为共振光散射探针,研究纳米铁-BSA反应体系测定生物大分子的最优条件及效果。[结果]纳米铁-BSA体系的最佳反应条件是pH值为7.4,纳米铁溶液的加入量为0.5ml,定量测定时选择吸收波长和发射波长均为477 nm。将配好的溶液放置35 min后再进行测定稳定性较好。在上述优化条件下,用该体系测定BSA的线性范围在0.07~0.60μg/ml,线性方程为IRLS=38.0+1583.3C(μg/ml),相关系数为0.99712,检出限为10.2 ng/ml。控制误差在5%以内,该体系对较高浓度的金属离子以及从1.0~100.0μg/ml浓度范围内的氨基酸有很强的抗干扰能力。[结论]该方法简便、快速、可靠且灵敏度高,可用于实际样品的测定。     

氯化钡共振瑞利散射法测定蜂蜜中硫酸链霉素残留

在0.05 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.     

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．     

曙红Y-盐酸丁卡因体系的共振瑞利散射光谱及其分析应用

在弱酸性介质中, 盐酸丁卡因(TA·HCl)与曙红Y形成1∶1的离子缔合物, 引起溶液共振瑞利散射(RRS)显著增强, 最大散射峰位于279 nm, 在一定范围内TA·HCl浓度与散射增强程度(ΔI)成正比, 可用于TA·HCl的测定;反应有很高的灵敏度, 对TA·HCl的检出限(3σ)为0.005 μg/mL;考察了共存物质的影响, 表明方法有良好的选择性. 基于TA·HCl与曙红Y反应产物的RRS光谱, 发展了一种高灵敏、简便快速测定痕量TA·HCl的新方法. 用于人血清和尿液中TA·HCl测定, 平均回收率94.7%～103.3%之间.     

曙红Y-盐酸丁卡因体系的共振瑞利散射光谱及其分析应用

在弱酸性介质中, 盐酸丁卡因(TA·HCl)与曙红Y形成1∶1的离子缔合物, 引起溶液共振瑞利散射(RRS)显著增强, 最大散射峰位于279 nm, 在一定范围内TA·HCl浓度与散射增强程度(ΔI)成正比, 可用于TA·HCl的测定;反应有很高的灵敏度, 对TA·HCl的检出限(3σ)为0.005 μg/mL;考察了共存物质的影响, 表明方法有良好的选择性. 基于TA·HCl与曙红Y反应产物的RRS光谱, 发展了一种高灵敏、简便快速测定痕量TA·HCl的新方法. 用于人血清和尿液中TA·HCl测定, 平均回收率94.7%～103.3%之间.