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1.
A novel method is used for the determination of some aminoglycoside antibiotics (AGs) such as etimicin (ETM), isepamicin (ISP) and amikacin (AMK). It is based on the resonance Rayleigh scattering (RRS) intensities enhanced by AGs‐induced CdTe quantum dots aggregation. Under the optimum conditions, the increments in RRS intensity were directly proportional to the concentration of AGs in certain ranges. At the same time, the second‐order scattering, the frequency‐doubling scattering and the frequency‐trebling scattering intensities were also enhanced and their increments were proportional to the concentration of AGs. Among them, the RRS method had the highest sensitivity; the linear ranges and detection limits for ETM, ISP and AMK were 0.085–7.2, 0.0067–1.2, 0.017–6.0 and 0.025, 0.0051, 0.0020 μg mL?1. This method was applied to the measurement of AGs in human serum and urine with satisfactory results. In addition, the reaction mechanism and the reasons for the enhancement of RRS are discussed using fluorescence, RRS, transmission electron microscope technology and quantum chemistry method. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

2.
Using AgNO3 as the precursor, stable silver nanochain (AgNC) sols, orange‐red in color, were prepared using hydrazine hydrate. A strong surface plasmon resonance Rayleigh scattering (RRS) peak occurred at 420 nm plus two surface plasmon resonance (SPR) absorption peaks at 410 nm and 510 nm. Rhodamine S (RhS) cationic dye was absorbed on the as‐prepared AgNC substrate to obtain a RhS–AgNC surface‐enhanced Raman scattering (SERS) nanoprobe that exhibited a strong SERS peak at 1506 cm–1 and a strong RRS peak at 375 nm. Upon addition of the analyte sodium hexametaphosphate (HP), it reacted with RhS, which resulted in a decrease in the SERS and RRS peaks that was studied in detail. The decreased SERS and RRS intensities correlated linearly with HP concentration in the range of 0.0125–0.3 µmol/L and 0.05–1.0 µmol/L, with a detection limit of 6 nmol/L and 20 nmol/L HP respectively. Due to advantages of high sensitivity, good selectivity and simple operation, the RhS molecular probes were used to determine HP concentration in real samples. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

3.
In pH 4.99‐6.06 Britton‐Robinson (BR) buffer medium, 6‐benzylaminopurine (6‐BA) reacted with Na2WO4 to form 1:1 anionic chelate (6‐BA·WO4)2‐, which further reacted with rhodamine 6G to form ternary ion complexes at room temperature. This resulted in a significant enhancement of resonance Rayleigh scattering (RRS) with a maximum RRS wavelength of 316 nm. Meanwhile, the fluorescence of the solution was quenched and excitation (λex) and emission (λem) wavelengths of the fluorescence were 290 and 559 nm, respectively. Intensities of RRS enhancing (ΔIRRS) and fluorescence quenching (ΔIF) were directly proportional to concentrations of 6‐BA. As a result, RRS and fluorescence quenching for determination of trace amounts of 6‐BA were developed. Under optimal conditions, linear ranges and detection limits of the two methods were 0.05‐15.00 µg/mL and 8.2 ng/mL (RRS), 0.50‐15.00 µg/mL and 17.0 ng/mL, respectively. It was found that the RRS method was superior to fluorescence quenching. The influence of these methods were investigated and results showed that RRS had good selectivity. RRS was applied to determine 6‐BA in vegetable samples with satisfactory results. Furthermore, the reaction mechanisms of the ternary ion‐association system are discussed. In addition, the polarization experiment revealed that the resonance light scattering (RLS) peak of Na2WO4‐6‐BA‐R6G consisted mainly of depolarized resonance fluorescence and resonance scattering. It was speculated that light emission fluorescence energy (EL) transformed into resonance light scattering energy (ERLS), which was a key reason for enhancement of RRS. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

4.
In weak acid medium, aluminum(III) can react with chlorophosphonazo III [CPA(III), H8L] to form a 1:1 coordination anion [Al(OH)(H4L)]2‐. At the same time, proteins such as bovine serum albumin (BSA), lysozyme (Lyso) and human serum albumin (HSA) existed as large cations with positive charges, which further combined with [Al(OH)(H4L)]2‐ to form a 1:4 chelate. This resulted in significant enhancement of resonance Rayleigh scattering (RRS), second‐order scattering (SOS) and frequency doubling scattering (FDS). In this study, we investigated the interaction between [Al(OH)(H4L)]2‐ and proteins, optimization of the reaction conditions and the spectral characteristics of RRS, SOS and FDS. The maximum RRS wavelengths of different protein systems were located at 357–370 nm. The maximum SOS and FDS wavelengths were located at 546 and 389 nm, respectively. The scattering intensities (ΔI) of the three methods were proportional to the concentration of the proteins, within certain ranges, and the detection limits of the most sensitive RRS method were 2.6–9.3 ng/mL. Moreover, the chelate reaction mechanism or the reasons for the enhancement of RRS were discussed through absorption spectra, fluorescence spectra and circular dichroism (CD) spectra. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   

5.
A new system for the determination of nucleic acid by rare earth metallic porphyrin of [tetra‐(3‐methoxy‐4‐hydroxyphenyl)]–Tb3+ [T(3‐MO‐4HP)–Tb3+] porphyrin as fluorescence spectral probe has been developed in this paper. Nucleic acid can enhance the fluorescence intensity of the T(3‐MO‐4HP)–Tb3+ porphyrin in the presence of bis(2‐ethylhexyl)sulfosuccinate sodium salt(AOT) micelle. In pH 8.00 Tris–HCl buffer solution, under optimum conditions, the enhanced fluorescence intensity is in proportion to the concentration of nucleic acids in the range of 0.05–3.00 µg mL?1 for calf thymus DNA (ct DNA) and 0.03–4.80 µg mL?1 for fish sperm DNA(fs DNA). Their detection limits are 0.03 and 0.01 µg mL?1, respectively. In addition, the binding interaction mechanism between T(3‐MO‐4HP)–Tb3+ porphyrin and ct DNA is also investigated by resonance scattering and fluorescence spectra. The maximum binding number is calculated by molar ratio method. The new system can be used for the determination of nucleic acid in pig liver, yielding satisfactory results. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

6.
In an acid medium solution, proteins such as bovine serum albumin, human serum albumin, ovalbumin, hemoglobin, lysozyme, γ‐globulin, α‐chymotrypsin and papain could react with [PdI4]2? by virtue of electrostatic attraction and hydrophobic force to form ion‐association complexes. As a result, the resonance Rayleigh scattering (RRS) and resonance nonlinear scattering such as second‐order scattering (SOS) and frequency doubling scattering (FDS) intensities were enhanced greatly and new scattering spectra appeared. The maximum scattering peaks of RRS, SOS and FDS were at 367, 720 and 370 nm, respectively. The enhanced RRS, SOS and FDS intensities were directly proportional to the concentrations of proteins. The detection limits for the different proteins were 2.4–11.8 ng/mL for RRS method, 9.5–47.9 ng/mL for SOS method and 4.6–18.5 ng/mL for FDS method. In this work, the influences of the interaction of [PdI4]2? with proteins on spectral characteristics of RRS, SOS and FDS were investigated and the optimum conditions were tested. Meanwhile, the effects of coexisting substances were tested and the results showed that the method exhibited a good selectivity. Based on the above research, a highly sensitive, simple and rapid method for the determination of trace amounts of proteins by resonance light scattering technique has been developed. It can be applied to the determination of proteins in tablet, human serum and urine samples. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

7.
We report a flow‐injection biosensor system with a capacitive transducer for assay and quality control of human immunoglobulin G (hIgG). The sensing platform is based on self‐assembled monolayers (SAMs) of carboxylic acid terminated alkyl‐thiols with covalently attached concanavalin A. The electrochemical characteristics of the sensor surface were assessed by cyclic voltammetry using a permeable redox couple (potassium ferricyanide). The developed biosensor proved capable of performing a sensitive label‐free assay of hIgG with a detection limit of 1.0 µg mL?1. The capacitance response depended linearly on hIgG concentration over the range from 5.0 to 100 µg mL?1, in a logarithmic plot. Typical measurements were performed in 15 min and up to 18 successive assays were achieved without significant loss of sensitivity using a single electrode. In addition, the biosensor can detect hIgG aggregates with concentrations as low as 0.01% of the total hIgG content (5.0 µg mL?1). Hence, it represents a potential post‐size‐exclusion chromatography–UV (post‐SEC–UV) binding assay for in‐process quality control of hIgG, which cannot be detected by SEC–UV singly at concentrations below 0.3% of the total hIgG content. Biotechnol. Bioeng. 2009; 104: 312–320 © 2009 Wiley Periodicals, Inc.  相似文献   

8.
At pH 1.3–1.6, tungstate WO42–, can be converted to hexatungstate W6O192–, which can react with positively charged polymyxin B sulfate (PMB) to result in enhancement of resonance Rayleigh scattering (RRS) and resonance non‐linear scattering, including second order scattering and frequency doubling scattering. Linear relationships can be established between enhanced scattering intensity and PMB concentration. The detection limits (3σ) were 5.5 ng/mL (RRS), 10.1 ng/mL (second order scattering) and 34.6 ng/mL (frequency doubling scattering). The optimum reaction conditions, influencing factors and related analytical properties were tested. The interaction mechanism was investigated via absorption spectrum, circular dichroism spectra and atomic force microscopy imaging. The basis of scattering enhancement is discussed. PMB in eardrops, human serum and urine, were quantified satisfactorily by RRS. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   

9.
In pH 5.0–5.4 HAc–NaAc buffer solution, lincomycin (Linco) reacted with Pd(II) to form 1:1 cationic chelate, which could further react with erythrosine (Ery) to form 1:1 ion‐association complexes (Pd–Linco)Ery. As a result, not only were the absorption and fluorescence spectra changed, but also the resonance Rayleigh scattering (RRS) intensity was greatly enhanced. These phenomena offered useful means for the determination of Linco by spectrophotometry, fluorescence and RRS methods. The linear range and detection limit of Linco were 0.20–3.00 µg/mL and 0.057 µg/mL, 0.20–4.80 µg/mL and 0.061 µg/mL, 0.05–2.70 µg/mL and 0.015 µg/mL for the spectrophotometric, fluorescence quenching and RRS methods, respectively. Among these, the RRS method obtained the highest sensitivity. Therefore, the optimum reaction conditions and the influences of coexisting substances were investigated using the RRS method. A simple, sensitive and rapid method has been developed for the determination of Linco in either the pharmaceutical form or human body fluids, and the reasons for RRS enhancement are discussed. Copyright © 2008 John Wiley & Sons, Ltd.  相似文献   

10.
Rapid and simple isocratic high‐performance liquid chromatographic methods with UV detection were developed and validated for the direct resolution of racemic mixtures of hyoscyamine sulfate and zopiclone. The method involved the use of αl‐acid glycoprotein (AGP) as chiral stationary phase. The stereochemical separation factor (?) and the stereochemical resolution factor (Rs) obtained were 1.29 and 1.60 for hyoscyamine sulfate and 1.47 and 2.45 for zopiclone, respectively. The method was used for determination of chiral switching (eutomer) isomers: S‐hyoscyamine sulfate and eszopiclone. Several mobile phase parameters were investigated for controlling enantioselective retention and resolution on the chiral AGP column. The influence of mobile phase, concentration and type of uncharged organic modifier, ionic strength, and column temperature on enantioselectivity were studied. Calibration curves were linear in the ranges of 1–10 µg mL‐1 and 0.5–5 µg mL‐1 for S‐hyoscyamine sulfate and eszopiclone, respectively. The method is specific and sensitive, with lower limits of detection and quantifications of 0.156, 0.515 and 0.106, 0.349 for S‐hyoscyamine sulfate and eszopiclone, respectively. The method was used to identify quantitatively the enantiomers profile of the racemic mixtures of the studied drugs in their pharmaceutical preparations. Thermodynamic studies were performed to calculate the enthalpic ΔH and entropic ΔS terms. The results showed that enantiomer separation of the studied drugs were an enthalpic process. Chirality 28:49–57, 2016. © 2015 Wiley Periodicals, Inc.  相似文献   

11.
In pH 4.0 Britton–Robinson buffer medium, PdCl2 was able to react with enzymes (EZ) such as lysozyme (LYSO) and papain (PAP) to form a coordination complex (EZ–PdCl2), which further reacted with MoO42‐ to form a ternary complex (MoO42‐–EZ–PdCl2). As a result, the absorption and fluorescence spectra changed; new spectra of resonance Rayleigh scattering (RRS), second‐order scattering (SOS) and frequency‐doubling scattering (FDS) appeared and their intensities were enhanced greatly. The maximum RRS, SOS and FDS wavelengths of two ternary complexes were located at 310, 560 and 350 nm, respectively. The increments of scattering intensity were directly proportional to the concentrations of EZ within certain ranges. The detection limits (3σ) of LYSO and PAP were 4.5 and 14.0 ng/mL (RRS method), 9.6 and 57.8 ng/mL (SOS method), and 5.2 and 106.0 ng/mL (FDS method). Taking the MoO42‐–LYSO–PdCl2 system, which was more sensitive, as an example, the effects of coexisting substances were evaluated. The methods showed excellent selectivity. Accordingly, new rapid, convenient, sensitive and selective scattering methods for the determination of LYSO and PAP were proposed and applied to determine LYSO in egg white with satisfactory results. The reaction mechanism and basis of the enhancement of scattering were discussed. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

12.
Sensitivity to azoxystrobin and kresoxim‐methyl of 80 single‐spore isolates of Magnaporthe oryzae was determined. The EC50 values for azoxystrobin and kresoxim‐methyl in inhibiting mycelial growth of the 80 M. oryzae isolates were 0.006–0.056 and 0.024–0.287 µg mL?1, respectively. The EC50 values for azoxystrobin and kresoxim‐methyl in inhibiting conidial germination of the M. oryzae populations were 0.004–0.051 and 0.012–0.105 µg mL?1, respectively. There was significant difference in sensitivity to azoxystrobin or kresoxim‐methyl between the tested isolates representing differential sensitivity to carbendazim (MBC) and kitazin P (IBP); however, there was no correlation between this difference in sensitivity to azoxystrobin or kresoxim‐methyl and sensitivity to MBC or IBP, indicating that there was no cross‐resistance between azoxystrobin or kresoxim‐methyl and MBC or IBP. In the protective and curative experiments, kresoxim‐methyl exhibited higher protective and curative activity than azoxystrobin when applied at 150 and 250 µg mL?1 accordingly, while azoxystrobin exhibited stronger inhibitory activity against M. oryzae isolates than that of kresoxim‐methyl in the in vitro test. The results of field experiments also suggested that both azoxystrobin and kresoxim‐methyl at 187.5 g.a.i. ha?1 gave over 73% control efficacy in both sites, exhibiting excellent activity against rice blast. Taken together, azoxystrobin and kresoxim‐methyl could be a good substitute for MBC or IBP for controlling rice blast in China, but should be carefully used as they were both at‐risk.  相似文献   

13.
Graphite oxide (GO) was prepared by the Hummer procedure, and can be dispersed to stable colloid solution by ultrasonic wave. The GO exhibited an absorption peak at 313 nm, and a resonance Rayleigh scattering (RRS) peak at 490 nm. In pH 4.6 HAc‐NaAc buffer solution, human serum albumin (HSA) combined with GO probe to form large HSA‐GO particles that caused the RRS peak increasing at 490 nm. The increased RRS intensity was linear to HSA concentration in the range 0.50–200 µg/mL. Thus, a new and simple RRS method was proposed for the determination of HSA in samples, with a recovery of 98.1–104%. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

14.
A sensitive spectrofluorimetric method using constant‐energy synchronous fluorescence technique is proposed for the determination of human albumin without separation. In this method, no reagent was used for enhancement of the fluorescence signal of albumin in the solution. Effects of some parameters, such as energy difference between excitation and emission monochromators (ΔE), emission and excitation slit widths and scan rate of wavelength were studied and the optimum conditions were established. For this purpose factorial design and response surface method were employed for optimization of the effective parameters on the fluorescence signal. The results showed that the scan rate of the wavelength has no significant effect on the analytical signal. The calibration curve was linear in the range 0.1–220.0 µg mL–1 of albumin with a detection limit of 7.0 × 10–3 µg mL–1. The relative standard deviations (RSD) for six replicate measurements of albumin were calculated as 2.2%, 1.7% and 1.3% for 0.5, 10.0 and 100.0 µg mL–1 albumin, respectively. Furthermore the proposed method has been employed for the determination of albumin in human serum and urine samples. Copyright © 2014 John Wiley & Sons, Ltd.  相似文献   

15.
Clotrimazole (CTZ) and cyclodextrin (CD) inclusion complexes having improved apparent water solubility were obtained from phase solubility diagrams. β‐CD (1.5% w/w) and hydroxypropyl‐β‐CD (40% w/w) offered poor CTZ solubility enhancements (12 and 384 times, respectively). Unexpectedly, the apparent solubility of CTZ was 9980 times increased from 0.4 µg.mL?1 (1.42 μM) without CD to 4.89 mg.mL?1 (14.9 mM) using randomly‐methylated β‐CD (Me‐β‐CD) (40% w/w). This is the highest apparent CTZ solubility improvement ever reported in the literature using conventional CDs. Quantitative nuclear magnetic resonance (1H‐NMR) coupled with two‐dimensional nuclear Overhauser effect (NOESY) experiments and molecular docking calculations showed that the highest interactions with Me‐β‐CD were reported for CTZ two phenyl groups. A lower interaction was reported for chlorophenyl, while imidazole had the weakest interaction with Me‐β‐CD. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

16.
Two simple, rapid, sensitive and precise spectrophotometric and spectrofluorimetric methods were developed for the determination of indacaterol maleate in bulk powder and capsules. Both methods were based on the direct measurement of the drug in methanol. In the spectrophotometric merthod (Method I) the absorbance was measured at 259 nm. The absorbance‐concentration plot was rectilinear over the range 1.0–10.0 µg mL?1 with a lower detection limit (LOD) of 0.078 µg mL?1 and lower quantification limit (LOQ) of 0.238 µg mL?1. Meanwhile in the spectrofluorimetric method (Method II) the native fluorescence was measured at 358 nm after excitation at 258 nm. The fluorescence‐concentration plot was rectilinear over the range of 1.0–40.0 ng mL?1 with an LOD of 0.075 ng mL?1and an LOQ of 0.226 ng mL?1. The proposed methods were successfully applied to the determination of indacaterol maleate in capsules with average percent recoveries ± RSD% of 99.94 ± 0.96 for Method I and 99.97 ± 0.81 for Method II. In addition, the proposed methods were extended to a content uniformity test according to the United States Pharmacopoeia (USP) guidelines and were accurate, precise for the capsules studied with acceptance value 3.98 for Method I and 2.616 for Method II. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

17.
Nearly all implantable bioelectronics are powered by bulky batteries which limit device miniaturization and lifespan. Moreover, batteries contain toxic materials and electrolytes that can be dangerous if leakage occurs. Herein, an approach to fabricate implantable protein‐based bioelectrochemical capacitors (bECs) employing new nanocomposite heterostructures in which 2D reduced graphene oxide sheets are interlayered with chemically modified mammalian proteins, while utilizing biological fluids as electrolytes is described. This protein‐modified reduced graphene oxide nanocomposite material shows no toxicity to mouse embryo fibroblasts and COS‐7 cell cultures at a high concentration of 1600 µg mL?1 which is 160 times higher than those used in bECs, unlike the unmodified graphene oxide which caused toxic cell damage even at low doses of 10 µg mL?1. The bEC devices are 1 µm thick, fully flexible, and have high energy density comparable to that of lithium thin film batteries. COS‐7 cell culture is not affected by long‐term exposure to encapsulated bECs over 4 d of continuous charge/discharge cycles. These bECs are unique, protein‐based devices, use serum as electrolyte, and have the potential to power a new generation of long‐life, miniaturized implantable devices.  相似文献   

18.
Zeying He  Yi Peng  Lu Wang  Ming Luo  Xiaowei Liu 《Chirality》2015,27(12):958-964
In this research, 10 chiral pesticides in fruits and vegetables were simultaneously determined using chiral liquid chromatography triple quadrupole‐linear ion trap hybrid mass spectrometry (LC‐QqLIT). The QuEChERS method was applied for sample preparation, and an enhanced product ion (EPI) scan was used to acquire tandem mass spectrometry (MS/MS) spectra for the library search. Parameters including limit of detection (LOD), limit of quantification (LOQ), linearity, relative standard deviation (RSD), and matrix effects were evaluated in five representative matrices (strawberry, leek, cowpea, tomato, and eggplant). Good linearity with coefficient of determination (r2) ≥0.997 was obtained for all 20 enantiomers in these five matrices over the range from 1.0 to 250 µg L‐1. All the recoveries at 5 and 50 µg kg‐1 (n = 5) ranged between 70% and 120% with RSD below 20%, indicating satisfactory precision. The LOQ for the enantiomers ranged between 0.05 and 1 µg kg‐1. Based on the proposed method, 135 commonly consumed fruits and vegetables taken from markets in Guizhou province, China, were analyzed. Enantioselective degradation for the selected chiral pesticides was observed in most of the positive samples. Chirality 27:958–964, 2015. © 2015 Wiley Periodicals, Inc.  相似文献   

19.
In this paper, a simple and novel method for the determination of polychlorinated biphenyls (PCBs), using silver nanoparticles (AgNPs) as a resonance light scattering (RLS) probe, is proposed. Under optimized conditions, there existed linear relationships between the enhancing RLS intensity of the system and the concentrations of PCBs in the range 8.0 × 10?8?1.0 × 10?6 g mL?1 for 2,4,4′‐trichlorbiphenyl (PCB28), 9.0 × 10?8?1.0 × 10?6 g mL?1 for 2,2′,5,5′‐tetrachlorbiphenyl (PCB52) and 4.0 × 10?8?1.0 × 10?6 g mL?1 for 3,3′,4,4′‐tetrachlorobiphenyl (PCB77). The corresponding detection limits (S/N = 3) were 2.6 × 10?8 g mL?1 for PCB28, 3.3 × 10?8 g mL?1 for PCB52 and 6.3 × 10?9 g mL?1 for PCB77, respectively. Finally, the mechanism of RLS enhancement was also studied. The results indicated that PCBs were adsorbed on the surface of AgNPs to form larger AgNP–PCB aggregates, resulting in the RLS enhancement of the system. Copyright © 2011 John Wiley & Sons, Ltd.  相似文献   

20.
In the present work, Fe3O4–carbon nanotubes (CNTs) composite was explored as a sensing material candidate for ammonium sulfide. Intense chemiluminescence emission can be observed during the catalytic oxidation of ammonium sulfide on the surface of Fe3O4–CNTs composite. Based on this phenomenon, a selective and sensitive gas sensor for the determination of ammonium sulfide was demonstrated. Under the optimized conditions, the linear range of cataluminescence intensity vs concentration of ammonium sulfide gas was 1.4–115 µg mL?1 (R = 0.998) with a limit of detection (S/N = 3) of 0.05 µg mL?1. The relative standard deviation (n = 5) for 14.3 µg mL?1 ammonium sulfide was 1.9%. There was no response to common foreign substances, such as sulfur dioxide, toluene, aether, ethanol, acetone, hydrogen sulfide, carbon bisulfide, benzene and ammonia. The proposed sensor was successfully applied for the determination of ammonium sulfide in artificial air samples. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

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