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Arsenic is a toxic metal element and the establishment of a highly sensitive and selective method for As has great significance to human health and environment protection. In sulfuric acid medium, As(â ¢) was reduced by NaBH4 to form AsH3 gas that was trapped by the Ce(â £)-I- catalytic absorption solution to cause Ce(â £) concentration decreased and As particle increased, which resulted in the resonance Rayleigh scattering (RRS) and fluorescence increased at 370 and 351 nm respectively. The increased RRS and fluorescence intensities were linear to As(â ¢) concentration in the range of 0.006~0.76 and 0.006~0.28 mg·L(-1) respectively, with a detection of As of 3.0 µg·L(-1). The new hydride generation-catalytic RRS method was applied for detection of trace As(â ¢) in milk samples, and the results were in agreement with that of hydride generation-atomic absorption spectrometry.
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Nanogold (NG) was prepared using NaBH4 reduction of HAuCl4. The NG was modified by the tobramycin-aptamer to obtain a stable Apt-NG probe for tobramycin. The three aptamers containing 15, 21 and 27 bases were examined, and results showed that the aptamer with 21 bases was best and was chosen for use. In pH 6. 8 PBS buffer solution and in the presence of NaCl, the Apt-GN probes were not aggregated. When tobramycin was added, it reacted with the Apt of Apt-NG probe to form a very stable Apt-Tbc complex and released NGs that were aggregated into big particles under the action of NaCl with three resonance Rayleigh scattering peaks at 285, 368 and 525 nm respectively. The resonance Rayleigh scattering peak increased at 368 nm due to the formation of big NG particles from the probe. The effect of pH buffer solution, its volume, and Apt-GN probe concentration on the ΔI value was considered. A 200 µL pH 6. 8 PBS buffer solution and 19. 1 nmol · L(-3) Apt-GN, giving max ΔI value, were chosen for use. Under the chosen conditions, the increased resonance Rayleigh scattering intensity ΔI368 nm was linear with Tbc concentration in the range of 1.9-58.3 ng mL(-3), with a regress equation of ΔI = 35.3c-23 and a detection limit of 0.8 ng · mL(-3) Tbc. A 10.0, 20.0 and 30.0 ng mL-3 Tbc was determined five times respectively, and the relative standard deviations were 6.8%, 5.0% and 4.4%. The influence of some foreign substances was examined on the determination of 38.9 ng · mL(-3) Tbc, within ±10% related error. Results showed that a 80 times of Zn2+, 40 times of L-glutamic acid, Cu2+, Mg2+ and Ca2+, 20 times of glucose and terramycin, 10 times of L-phenylalanine and glycin, 2 times of L-aspartic acid, and 6 times of bovine serum albumin (BSA) and human serum albumin (HSA) do not interfere with the RRS determination of Tbc. The results showed that this aptamer-nanogold RRS method is of good selectivity. Tbc in real sample was analyzed, and the analytical result was in agreement with that of reference results, with a relative standard deviation of 6.5%-7.6% and a recovery of 95.0%-107%.
Assuntos
Resíduos de Drogas/análise , Tobramicina/análise , Ouro , Nanopartículas MetálicasRESUMO
In pH 7.0 Na2HPO4-NaH2PO4 buffer solution, nanogold particles interacted with the aptamer to form a stable aptamer-nanogold complex that was not aggregation by NaCl. At 80 degrees C, K+ and aptamer folded to form a stable G-quadruplex that released nanogold particles, the uncombined nanogold particles aggregated to large nanogold clusters that caused the increase in resonance scattering (RS) intensity at 563 nm in high concentration of NaCl, and the laser scattering showed that the average diameter was 120 nm. In the present paper, the resonance scattering spectral characteristics of K+ -ssDNA1-Au, K+ -ssDNA2-Au and K+ -aptamer-Au systems were investigated, and the structural changes of aptamer were studied by circular dichroism spectral technology. Effects of pH value, NaCl concentration, nanogold concentration, aptamer concentration, and the reactation temperature and time on the resonance scattering intensity were considered in detail. The influence of coexistent substances on the determination of K+ was investigated, result showed that the common heavy metal ions such as Cu2+, Mg2+, Pb2+, Ca2+, Al3+, Zn2+ and Fe3+ do not interfere with the determination, and the method has good selectivity. Under the conditions selected, a 0. 67-3 350 micromol x L(-1) K+ can be detected by the aptamer-nanogold RS assay, with a detection limit of 0.3 micromol x L(-1) K+, regression equation deltaI = 0.167c-0.7, and a coefficient of 0.9932. The method was used for analysis of K+ in serum sample with the results consistent with the ion-selective electrode method.
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OBJECTIVE: To study the structure of the polysaccharides constituents in the fruits of Siraitia grosvenorii (Swingle) C. Jeffrey. METHODS: SGPS2 was purified by DEAE-cellulose and Sephadex G-200 column chromatography, the component and structure of SGPS2 were analyzed on the basis of spectral and chemical studies by HPLC, IR analysis, partial hydrolysis with acid, methylation analysis, GC and 13C-NMR. RESULTS: The molecular weight of SGPS2 was 650 000. Polysaccharide was composed of L- made up of (1 --> 2, 4) linked rhamnose, (1 --> 4) linked rhamnose residues in main chain; and (1 --> 2) linked rhamnose, (1 --> 3) linked rhamnose in side chains. Terminal residues attached main chain to rhamnose. CONCLUSION: SGPS2 was composed of rhamnose and curonic acid.
Assuntos
Cucurbitaceae/química , Frutas/química , Glucuronatos/análise , Polissacarídeos/química , Ramnose/análise , Cromatografia Líquida de Alta Pressão , Hidrólise , Espectroscopia de Ressonância Magnética , Estrutura Molecular , Peso Molecular , Plantas Medicinais/química , Polissacarídeos/isolamento & purificaçãoRESUMO
In acetate buffer solution and in the presence of glucose oxidase (GOD), glucose reduced the dissolved oxygen to form H2O2 that oxidized catalytically the excess KI to from I3- by horseradish peroxidase (HRP). The I3- combines respectively with rhodamine S (RhS), rhodamine 6G(Rh6G), butyl-rhodamine B(b-RhB) and rhodamine B(RhB) to form RhS-I3, Rh6G-I3, b-RhB-I3 and RhB-I3 associated particles that result in fluorescence quenching at 556, 556, 584 and 584 nm, respectively. Under the optimal conditions, the concentration of glucose in the range of 0.083-9.99, 0.17-8.33, 0.33-8.33 and 0.33-9.99 micromol x L(-1) is linear with their fluorescence quenching at 556, 556, 584 and 584 nm, with detection limits of 0.059, 0.17, 0.21 and 0.16 micromol x L(-1) glucose. And the regression equation was deltaF = 40.0c + 3.0, deltaF = 23.9c + 8.1, deltaF = 25.6c + 4.2, and deltaAF = 18.4c + 0.8, respectively. The RhS system was the most sensitive and stable, and was chosen for use. Influence of some foreign substances on the RhS fluorescence quenching determination of 6.67 micromol x L(-1) glucose was examined, with a relative error of +/- 10%. Results showed that 1000-fold Mg2+ and Cu2+, 300-fold Mn2+, 100-fold Zn2+, Al3+ and Co2+, 60-fold L-tyrosine, urea and nicotinic acid, 50-fold Fe3+, HSA and BSA, 10-fold sucrose, vitamin B2, L-lysine, L-glutamic acid and L-cystine did not interfere with the determination. This RhS fluorescence quenching assay was applied to the determination of glucose in the serum samples with satisfactory results.
Assuntos
Glucose Oxidase , Glucose/análise , Peroxidase do Rábano Silvestre , Cistina , Fluorescência , Ácido Glutâmico , Peróxido de Hidrogênio , Lisina , Oxirredução , Rodaminas , Espectrometria de Fluorescência , TirosinaRESUMO
The nano-photochemical reaction of polyethyelene glycol (PEG)-Au3+ was studied by resonance scattering and absorption spectrophotometry, and transmission electron microscopy. Influence of various factors on the preparation of gold nanoparticles was considered. There is a correlation between the molecular mass of PEG and the size of gold nanoparticles. A new photochemical method was proposed for the preparation of gold nanoparticles in size of 6-60 nm, using different molecular mass of PEG. The cause of obtaining gold nanoparticle with different size is the different space effect and hydrophobic property of PEG. A reasonable nano-reaction mechanism was developed.