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1.
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.  相似文献   

2.
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.  相似文献   

3.
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%.  相似文献   

4.
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.  相似文献   

5.
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.  相似文献   

6.
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.  相似文献   

7.
采用高效液相色谱法同时测定了口服液中的咖啡酸和阿魏酸含量,用Shim-pack VP-ODS柱(150 mm×4.6 mm,0.3μm),流动相:乙腈-3%的冰醋酸水溶液(体积比为11∶89),流速:1.0 mL/min,检测波长:321 nm.咖啡酸和阿魏酸的浓度与峰面积呈良好的线性关系,其线性范围分别为0.126～63.0 μg/mL(r=0.999 7)和0.120～24.0 μg/mL(r=0.999 9),平均回收率(n=3)分别为100.7%和99.9%,相对标准偏差(RSD)分别为2.11%和2.12%,检出限分别为42 ng/mL和43 ng/mL,样品中咖啡酸和阿魏酸的平均含量分别为3.26μg/mL和2.36μg/mL.
Abstract：
An HPLC method was established for the simultaneous determination of ferulic acid and caffeic acid in oral liquid. The Shim-pack VP-ODS column (150 mm×4.6 mm, 0.3 μm) was used with a mobile were detected at a wavelength of 321 nm. The flow rate was 1.0 mL/min and the injection volume was 20 μL. The calibration curve was linear in the range of 0. 126-63.0 μg/mL (r=0. 999 7) for caffeic acid and 0. 120-24.0 μg/mL (r=0. 999 9) for ferulic acid. The average recovery (n=3) was 100.7% with RSD 2. 11% for caffeic acid and was 99.9% with RSD 2.12% for ferulic acid. The detection limit was 42 ng/mL for caffeic acid and 43 ng/mL for ferulic acid. The average content of the samples was 3. 26 μg/mL for caffeic acid and 2.36 μg/mL for ferulic acid.  相似文献   

8.
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.  相似文献   

9.
在酸性条件下,氢溴酸加兰他敏被质子化后与AuCl4-形成离子缔合物被二氯甲烷所萃取,当缔合物被带入含鲁米诺的氯化十六烷基三甲基铵(Cetyltrimethylammonium Chlorine,CTAC)逆胶束纳米微反应器中时,离解出来的AuCl4-与鲁米诺产生化学发光.发光强度与氢溴酸加兰他敏的含量呈线性关系,从而可间接测定氢溴酸加兰他敏的含量.在优化的试验条件下,线性范围为0.001～15 μg/mL,检出限(3σ)为0.05 ng/mL,对浓度为1.0 μg/mL的氢溴酸加兰他敏进行11次平行测定,相对标准偏差(RSD)为2.24%.该法已成功用于片剂、针剂和生物体液中氢溴酸加兰他敏的测定.
Abstract：
Under the acidic condition, galantamine hydrobromide was protonated and formed an ion-complex with the negative ion AuCl4-, and the ion-complex was extracted by dichloromethane. When the ioncomplex entered a reversed micellar nanometer microreactor of cetyltrimethylammonium chlorine containing luminol, the dissociated AuCl4- reacted with luminol and produced an analytical chemiluminescnece signal. Under the optimum conditions, the CL response was linear to galantamine hydrobromide concentration ranging from 0. 001 to 15 g/mL and the limit of detection was 0.05 ng/mL with a relative standard deviation (n=11) of 2.24% for 1.0 g/mL galantamine hydrobromide. The method has been successfully applied to the determination of the studied drug in tablets, injections and biological fluids.  相似文献   

10.
A method was developed for the simultaneous determination of four kinds of estrogens(hexoestrol, diethylstilbestrol, estrone, and 17-beta-estradiol) in feed by gas chromatography-mass spectrometry(GC-MS). After the sample was extracted by ethyl ether and cleaned-up on HLB phase extraction column, four kinds of estrogens were derived and quantified in gas chromatographymass spectrometry. The results showed that the linear detectable ranged from 2.5 ng·mL~(-1) to 250 ng·mL~(-1) for hexoestrol and from 5 ng·mL~(-1) to 500 ng·mL~(-1) for three other estrogens with the correlation coefficients(R~2) were no less than 0.990. The recoveries were in the range of 76.34%-96.33% and the relative standard deviation was no more than 22.7%. The limits of quantitation(LOQ) for all analytics were between 10 ug·kg~(-1) and 20 ug·kg~(-1).The method was accurate and sensitive and could meet the actual requirements for the analyses of feed samples.  相似文献   

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