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1.
A nanocatalyst coating was prepared at surface of a glassy carbon electrode by electropolymerization of pyrrole by cycling the electrode potential between ?0.8 and 0.8 V (vs. Ag/AgCl). Then, polypyrrole film was potentiostatically coated with platinum nanoparticles at constant potential of ?0.2 V (vs. Ag/AgCl). The resulting electrode was denoted as GCE/PPy/Pt. This modified electrode was characterized by IR, SEM, TEM and EDX. The electrocatalytic oxidation of ethanol at the GCE/PPy/Pt has been investigated using cyclic voltammetric and chronoamperometric methods. The effects of various parameters on electrocatalytic oxidation of the ethanol, such as the thickness of PPy film, the amount of platinum nanoparticles, ethanol concentration, potential scan rate and working potential limit in anodic direction, were investigated. The kinetic of the ethanol oxidation is discussed on the GCE/PPy/Pt. The stability and reproducibility of this modified electrode were also studied.  相似文献   

2.
An electrochemical sensor for simultaneous determination of dopamine (DA), uric acid (UA), guanine (G), and adenine (A) has been constructed by copolymerizing melamine monomer and Ag ions on a glassy carbon electrode (GCE) with cyclic voltammetry. The poly-melamine and nano Ag formed a hybridized film on the surface of the GCE. The morphology of the film was characterized by scanning electron microscope. The electrochemical and electrocatalytic properties of this film were characterized by cyclic voltammetry, linear sweep voltammetry, and square wave voltammetry (SWV). In 0.1 M phosphate buffer solution (pH 4.5), the modified electrode resolved the electrochemical response of DA, UA, G, and A into four well-defined voltammetric oxidation peaks by SWV; the oxidation peak current of DA, UA, G, and A increased 13-, 6-, 7-, and 9-fold, respectively, compared with those at the bare GCE and the SWV peak currents of DA, UA, G, and A with linear concentrations in the ranges of 0.1–50, 0.1–50, 0.1–50, and 0.1–60 μM, respectively. Based on this, a method for simultaneous determination of these species in mixture was setup. The detection limits were 10 nM for DA, 100 nM for UA, 8 nM for G, and 8 nM for A.  相似文献   

3.
The authors describe a dopamine (DA) sensor based on a glassy carbon electrode modified with a composite film composed of carbon dots (C-dots) and graphene functionalized with an ionic liquid. The C-dots were functionalized with carboxy groups whose negative charge promotes electrostatic attraction to the protonated amino groups in DA. The presence of an imidazole cation in the IL facilitates interaction with the C-dots and DA via electrostatic interactions and π-stacking forces. Under optimal conditions, the modified GCE display improved electrochemical response to DA compared to a bare GCE, or a GCE modified with C-dots or IL-graphene only. The oxidation current, measured best at a potential of 0.22 V (vs. Ag/AgCl) is linearly related to the DA concentration in the 0.1 to 600 μM range, with a 30 nM detection limit at a signal-to-noise ratio of 3. Ascorbic acid does not interfere even in large excess, and the sensor is stable for at least a month. The modified GCE was applied to the determination of DA in spiked fetal bovine serum and gave satisfactory results.  相似文献   

4.
A glassy carbon electrode (GCE) was anodically oxidized by cyclic voltammetry (CV) in 0.05 M sulfuric acid to introduce hydroxy groups on its surface (GCEox). Next, an imidazolium alkoxysilane (ImAS) is covalently tethered to the surface of the GCEox via silane chemistry. This electrode is further modified with graphene oxide (GO) which, dispersed in water, spontaneously assembles on the electrode surface through electrostatic interaction and π-interaction to give an electrode of type GO/ImAS/GCE. Electroreduction of GO and GCEox by CV yields electroreduced GO (erGO) and an electrode of the type erGO/ImAS/GCE. This electrode displays excellent electrocatalytic activity for the oxidation of ascorbic acid (AA), dopamine (DA) and uric acid (UA). Three fully resolved anodic peaks (at ?50 mV, 150 mV and 280 mV vs. Ag/AgCl) are observed during differential pulse voltammetry (DPV). Under optimized conditions, the linear detection ranges are from 30 to 2000 μM for AA, from 20 to 490 μM for UA, and from 0.1 to 5 μM and from 5 μM to 200 μM (two linear ranges) for DA. The respective limits of detection (for an S/N of 3) are 10 μM, 5 μM and 0.03 μM. The GCE modified with erGO and ImAS performs better than a bare GCE or a GCE modified with ImAS only, and also outperforms many other reported electrodes for the three analytes. The method was successfully applied to simultaneous analysis of AA, DA and UA in spiked human urine.
Graphical abstract Differential pulse voltammetric simultaneous determination of ascorbic acid, dopamine and uric acid is achieved on a glassy carbon electrode modified with electroreduced graphene oxide and imidazolium groups, through anodic treatment of glassy carbon and silane chemistry.
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5.
DPPH (2,2-diphenyl-1-picrylhydrazil), a free radical-containing organic compound, is used widely to evaluate the antioxidant properties of plant constituents. Here, we report an efficient electroactive DPPH molecular system with excellent electrocatalytic sensor properties, which is clearly distinct from the traditional free radical-based quenching mechanism. This unusual molecular status was achieved by the electrochemical immobilization of graphene oxide (GO)-stabilized DPPH on a glassy carbon electrode (GCE). Potential cycling of the DPPH adsorbed-GCE/GO between ??1 and 1 V (Ag/AgCl) in a pH 7 solution revealed a stable and well-defined pair of redox peaks with a standard electrode potential, E0′?=?0?±?0.01 V (Ag/AgCl). Several electrochemical characterization studies as well as surface analysis of the GCE/GO@DPPH-modified electrode by transmission electron microscopy, Raman, and infrared spectroscopy collectively identified the imine/amine groups as the redox centers of the electroactive DPPH on GO. The use of different carbon-supports showed that only oxygen-functionalized GO and MWCNTs could provide major electroactivity for DPPH. This highlights the importance of a strong hydrogen-bonded network structure assisted by the concomitant π-π interactions between the organic moiety and oxygen function groups of carbon for the high electroactivity and stability of the GCE/GO@DPPH-NH/NH2-modified electrode. The developed electrode exhibited remarkable performance towards the electrocatalytic oxidation of NADH at 0 V (Ag/AgCl). The amperometric i-t sensing of NADH showed high sensitivity (488 nA μM?1 cm?2) and an extended linear range (50 to 450 μM) with complete freedom from several common biochemical/chemical interferents, such as ascorbic acid, hydrazine, glucose, cysteine, citric acid, nitrate, and uric acid.  相似文献   

6.
《Analytical letters》2012,45(12):2387-2403
Abstract

A detailed study of voltammetric behavior of ethiofencarb (ETF) is reported using glassy carbon electrode (GCE) and hanging mercury drop electrode (HMDE). With GCE, it is possible to verify that the oxidative mechanism is irreversible, independent of pH, and the maximum intensity current was observed at +1.20 V vs. AgCl/Ag at pH 1.9. A linear calibration line was obtained from 1.0×10?4 to 8.0×10?4 mol L?1 with SWV method. To complete the electrochemical knowledge of ETF pesticide, the reduction was also explored with HMDE. A well‐defined peak was observed at –1.00 V vs. AgCl/Ag in a large range of pH with higher signal at pH 7.0. Linearity was obtained in 4.2×10?6 and 9.4×10?6 mol L?1 ETF concentration range.

An immediate alkaline hydrolysis of ETF was executed, producing a phenolic compound (2‐ethylthiomethylphenol) (EMP), and the electrochemical activity of the product was examined. It was deduced that it is oxidized on GCE at +0.75 V vs. AgCl/Ag with a maximum peak intensity current at pH 3.2, but the compound had no reduction activity on HMDE.

Using the decrease of potential peak, a flow injection analysis (FIA) system was developed connected to an amperometric detector, enabling the determination of EMP over concentration range of 1.0×10?7 and 1.0×10?5 mol L?1 at a sampling rate of 60 h?1. The results provided by FIA methodology were performed by comparison with results from high‐performance liquid chromatography (HPLC) technique and demonstrated good agreement with relative deviations lower than 4%. Recovery trials were performed and the obtained values were between 98 and 104%.  相似文献   

7.
A new voltammetric sensor based on electropolymerization of glycine at glassy carbon electrode (GCE) was developed and applied to determine of pyrazinamide (PZA) by square-wave voltammetry (SWV). The initial cyclic voltammetric studies showed an electrocatalytic activity of poly(Gly)/GCE on redox system of pyrazinamide in 0.1 mol L?1 phosphate buffer solution pH 7.5, with E Pc and E Pa in ?0.85 and ?0.8 V (versus E Ag/AgCl), respectively. Studies at different scan rates suggest that the redox system of pyrazinamide at poly(Gly)/GCE is a process controlled by diffusion in the interval from 10 to 100 mV s?1. Square-wave voltammetry-optimized conditions showed a linear response of PZA concentrations in the range from 0.47 to 6.15 μmol L?1 (R?=?0.998) with a limit of detection (LOD) of 0.035 μmol L?1 and a limit of quantification (LOQ) of 0.12 μmol L?1. The developed SWV-poly(Gly)/GCE method provided a good intra-day (RSD?=?3.75 %) and inter-day repeatability (RSD?=?4.96 %) at 4.06 μmol L?1 PZA (n?=?10). No interference of matrix of real samples was observed in the voltammetric response of PZA, and the method was considered to be highly selective for the compound. In the accuracy test, the recovery was found in the range of 98.2 and 104.0 % for human urine samples and pharmaceutical formulation (tablets). The PZA quantification results in pharmaceutical tablets obtained by the proposed SWV-poly(Gly)/GCE method were comparable to those found by official analytical protocols.  相似文献   

8.
《Analytical letters》2012,45(3):459-470
Abstract

A highly sensitive electrochemical biosensor for the detection of trace amount of 1‐naphthol was designed. Acid‐denatured DNA were immobilized onto the pretreated glassy carbon electrode (GCE(ox)) surface. Two well‐defined oxidation peaks were observed on the denatured DNA‐modified GCE(ox) at about +0.80 V and +1.10 V (vs. Ag/AgCl) in 0.10‐M acetate buffer (pH 5.0). The peak current of the guanine residue decreased with increasing concentration of 1‐naphthol. The optimum experimental conditions for the detection of 1‐naphthol were explored, and the calibration was linear for 1‐naphthol in the range of 1.0×10?8?1.1×10?6 M, with a correlation coefficient of 0.998. The limit of detection (LOD) was 5.0×10?9 M (S/N=3).  相似文献   

9.
Li Zhang  Yonghong Ni  Hua Li 《Mikrochimica acta》2010,171(1-2):103-108
The direct electrocatalytic oxidation of glucose in alkaline medium at an electrode modified with microcubes of porous cuprous oxide is reported. Compared to the glassy carbon electrode, a substantial increase in the efficiency of the electrocatalytic oxidation of glucose is observed starting at around +0.20 V (vs. Ag/AgCl). The pH dependence of the response was examined by cyclic voltammetry. This non-enzymatic amperometric sensor may be used for non-enzymatic detection of glucose with a high and reproducible sensitivity of 10.95 μA per mM at a potential of +0.40 V, with response times of <3 s, a linear range from 2.0 to 350 μM, and a detection limit of 1.3 μM. The porous microcubes are conveniently prepared, and display high sensitivity and repeatability.  相似文献   

10.
Fei Li 《Talanta》2009,79(3):845-31
A simple and rapid method for morphine detection has been described based on electrochemical pretreatment of glassy carbon electrode (GCE) which was treated by anodic oxidation at 1.75 V, following potential cycling in the potential range from 0 V to 1.0 V vs. Ag|AgCl reference electrode. The sensitivity for morphine detection was improved greatly and the detection limit was 0.2 μM. The reproducibility of the voltammetric measurements was usually less than 3% RSD for six replicate measurements. Moreover, this method could readily discriminate morphine from codeine. And an electrochemical detection of morphine in spiked urine sample was succeeded with satisfactory results.  相似文献   

11.
The electrochemical oxidation of anticancer drug 5-fluorouracil (5-FU) at graphene oxides (GOs)/carbon nanotubes (CNTs) nanohybrid-modified screen-printed carbon and glassy carbon electrodes was studied by voltammetric techniques. The modified electrodes showed better performance toward the electro-oxidation and determination of 5-FU compared to CNTs-modified or GOs-modified electrodes. The oxidation peak current obtained at about + 1.156 V (vs. Ag/AgCl) from square wave voltammetry was linearly dependent on the 5-FU concentration in the ranges of 0.05–5 and 5–1200 µM in phosphate buffer solution of pH 7.0. The developed method was applied successfully to the electrochemical sensing of 5-FU in human plasma samples at micro-molar concentration levels with satisfactory results. It is hopeful that the developed method in the future can be used for the simple and fast determination of 5-FU in clinical test and pharmacokinetics.  相似文献   

12.
A thin film of poly(eriochrome black T) was deposited on the surface of glassy carbon electrode by cyclic voltammetry, and this system is shown to enable the sensitive determination of adenine (A) and guanine (G). Scanning electron microscopy, Fourier transform infrared spectroscopy and electrochemical impedance spectroscopy were carried out to characterize the film which exhibits excellent electrocatalytic activity toward the oxidation of A and G in 0.1 M phosphate buffer solution (pH 4.0). Square wave voltammetry reveals an oxidation peak at 1084 mV whose current is linearly related to the concentration of A in the range from 0.05 to 1.00 μM. The oxidation peak for G occurs at 788 mV, and its current is linearly related to the concentration of G in the range from 0.025 to 1.00 μM. The detection limits are 0.017 μM for A and 0.008 μM for G (at S/N?=?3), respectively. The modified electrode displays good reproducibility and selectivity for the determination of A and G. The sensor was applied to quantify A and G in fish sperm DNA with satisfactory results.
Figure
Square wave voltammograms of bare GCE (a), PEBT/GCE (b) in the presence of 1.00 μM adenine (A) and 1.00 μM guanine (G).  相似文献   

13.
A glassy carbon electrode (GCE) was modified with poly(L-arginine) (P-Arg), reduced graphene oxide (rGO) and gold nanoparticle (AuNP) to obtain an electrode for simultaneous determination of dopamine (DA), serotonin (5-HT) and L-tryptophan (L-Trp) in the presence of ascorbic acid (AA). The modified GCE was prepared via subsequent ‘layer-by-layer’ deposition using an electrochemical technique. The surface morphology of the modified electrode was studied by scanning electron microscopy, and electrochemical characterizations were carried out via cyclic voltammetry and electrochemical impedance spectroscopy. The modified electrode showed excellent electrocatalytic activity toward DA, 5-HT and L-Trp at pH 7.0. Figures of merit for the differential pulse voltammetric reponse are as follows: (a) Response to DA is linear in two intervals, viz. 1.0–50 nM and 1.0–50 μM DA concentration range, the typical working voltage is 202 mV (vs. Ag/AgCl), and the detection limit is 1 nM (at an S/N ratio of 3). For 5-HT, the respective data are 10 to 500 nM and 1.0 to 10 μM, 381 mV, and 30 nM. For L-Trp, the respective data are 10–70 nM and 10–100 μM, 719 mV, and 0.1 μM. The modified GCE is fairly selective. It was successfully applied to the simultaneous determination of DA, 5-HT, and L-Trp in spiked urine samples, and high recovery rates were found.
Graphical abstract Schematic presentation of the voltammetric sensor based on a glassy carbon electrode modified with poly(L-arginine), reduced graphene oxide (rGO) and gold nanoparticle (GCE/P-Arg/ErGO/AuNP) for simultaneous determination of dopamine (DA), serotonin (5-HT) and L-tryptophan (L-Trp).
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14.
Various carbon nanomaterials for use in anodic stripping voltammetric analysis of Hg(II), Cu(II), Pb(II) and Cd(II) are screened. Graphene, carbon nanotubes, carbon nanofibers and fullerene (C60), dispersed in chitosan (Chit) aqueous solution, are used to modify a glassy carbon electrode (GCE). The fullerene-chitosan modified GCE (C60-Chit/GCE) displays superior performance in terms of simultaneous determination of the above ions. The electrodes and materials are characterized by electrochemical impedance spectroscopy, cyclic voltammetry, scanning electron microscopy, Raman spectroscopy, X-ray diffraction and X-ray photoelectron spectroscopy. The excellent performance of C60-Chit/GCE is attributed to the good electrical conductivity, large surface area, strong adsorption affinity and unique crystalline structure of C60. Using differential pulse anodic stripping voltammetry, the assay has the following features for Hg(II), Cu(II), Pb(II) and Cd(II), respectively: (a) Peak voltages of +0.14, ?0.11, ?0.58 and???0.82 V (vs SCE); (b) linear ranges extending from 0.01–6.0 μM, 0.05–6.0 μM, 0.005–6.0 μM and 0.5–9.0 μM; and (c), detection limits (3σ method) of 3 nM (0.6 ppb), 14 nM (0.9 ppb), 1 nM (0.2 ppb) and 21 nM (2.4 ppb). Moreover, the modified GCE is well reproducible and suitable for long-term usage. The method was successfully applied to the simultaneous determination of these ions in spiked foodstuff.
Graphical abstract Compared with graphene, carbon nanotubes and carbon nanofibers, an electrode modified with fullerene in chitosan electrode displays superior performance for the simultaneous anodic stripping voltammetric detection of Hg(II), Cu(II), Pb(II) and Cd(II).
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15.
用循环伏安法制备银掺杂聚L-酪氨酸修饰玻碳电极,研究了多巴胺、肾上腺素和抗坏血酸在其电极上的电化学行为,建立了同时测定多巴胺、肾上腺素和抗坏血酸的新方法。当3种组分共存时,在磷酸盐缓冲溶液(pH6.0)中,扫描速率为140mV/s,多巴胺和肾上腺素在修饰电极上分别产生还原峰,峰电位分别为0.198和-0.205V,多巴胺和肾上腺素氧化峰重叠,峰电位为0.313V(vs.Ag/AgCl);抗坏血酸产生一个氧化峰,峰电位0.108V(vs.Ag/AgCl)。多巴胺和肾上腺素的ΔEpc=0.403V,抗坏血酸的氧化峰与多巴胺和肾上腺素的ΔEpa=0.205V,用还原峰和氧化峰可同时测定多巴胺、肾上腺素和抗坏血酸,3种组分同时测定的线性范围分别为5.0×10-6~1.0×10-4mol/L,8.0×10-6~1.0×10-4mol/L和3.0×10-5~1.0×10-3mol/L;检出限分别为5.0×10-7,8.0×10-7和5.0×10-6mol/L。本方法用于人尿液中多巴胺、肾上腺素和抗坏血酸的同时测定,结果满意。  相似文献   

16.
The electrochemical oxidation of the three fluoroquinolone drugs FQs: gatifloxacin GTF, moxifloxacin MXF and sparfloxacin SPF, at the bare and DNA‐modified glassy carbon electrodes has been studied by voltammetric techniques. The three FQs showed one irreversible oxidation peak at potential range 0.85–0.91 V vs. Ag‐AgCl, in phosphate buffer of pH 7.0. Differential pulse voltammetry (DPV) and UV‐absorption spectroscopic techniques were employed to probe the interaction between the FQs and calf thymus double stranded deoxyribonucleic acid (ds CT‐DNA). From electrochemical data, the binding constant between DNA and the gatifloxacin, moxifloxacin and sparfloxacin are calculated to be 3228, 2596 and 2857 M?1 respectively. Based on electrochemical and spectroscopic results, the mode of binding of fluoroquinolone to DNA through combined effect of intercalation and electrostatic interaction was concluded. A detection scheme based on a preconcentration and differential pulse voltammetric (DPV) determination at dsDNA modified glassy carbon electrode (DNA/GCE) was proposed for the trace determination of the studied analytes. The developed method was successfully applied to the determination of the FQs in pharmaceutical formulations.  相似文献   

17.
《Electroanalysis》2005,17(14):1309-1316
The detection limit (about 0.017 μg mL?1) for voltammetric determination of iodide (peak at +0.87 V vs. Ag/AgCl at pH 2) at a glutaraldehyde‐cross‐linked poly‐L ‐lysine modified glassy carbon electrode involving oxidation to iodine was found to be several orders of magnitude lower than that for the voltammetric determination on a bare glassy carbon electrode. This method was applied successfully to the determination of iodide in two medicinal formulations. Idoxuridine was determined indirectly at the same electrode by accumulating it first at ?0.8 V vs. Ag/AgCl. At this potential the C? I bond in the adsorbed idoxuridine is reduced giving iodide, which is then determined at the modified electrode. The method was successfully applied to the determination of idoxuridine in a urine sample.  相似文献   

18.
《Electroanalysis》2017,29(2):529-537
A glassy carbon electrode (GCE) coated with a thin film of organoattapulgite was used for the voltammetric detection and quantification of mangiferin (MG), a bioactive xanthone with several therapeutic properties. The used modified attapulgite was prepared by surface grafting of [3‐(2‐aminoethylamino)propyl]trimethoxysilane. The grafted clay was characterised by SEM, CHN elemental analysis, FTIR spectroscopy and XRD techniques. The electrochemical behaviour of MG was first investigated on bare GCE by cyclic voltammetry which showed a single irreversible oxidation peak at ca 0.770 V (vs Ag/AgCl) in HCl/KCl buffer at pH 1. When the GCE was covered by the organoattapulgite, the electrode response for MG increased significantly due to favourable electrostatic interactions between MG and the protonated organoclay. A sensitive voltammetric method for the determination of MG, based on adsorptive stripping voltammetry was then developed. A linear variation of MG concentration with peak current was obtained in the range from 0.61 to 10.57 μM, with a detection limit of 2.75×10−7 M (S/N=3). Kinetic and chronocoulometric studies were also performed to characterise the diffusion of MG at the organoclay modified electrode. The interfering effect of some compounds likely to affect the stripping signal of MG was also evaluated, followed by the application of the developed method to a real biological sample.  相似文献   

19.
Wang  Yong  Qu  Jianhang  Li  Shufang  Dong  Ying  Qu  Jianying 《Mikrochimica acta》2015,182(13):2277-2283

We describe an electrochemical sensor for simultaneous determination of hydroquinone (HQ) and catechol (CC). A glassy carbon electrode (GCE) was modified with gold nanoparticles, L-cysteine, and ZnS/NiS@ZnS quantum dots using a layer-by-layer technique. The materials were characterized by X-ray diffractometry, field emission scanning electron microscopy, and electrochemical impedance and Fourier transform infrared spectroscopy. Cyclic voltammetry and differential pulse voltammetry revealed this modified GCE to represent a highly sensitive sensor for the simultaneous determination of HQ and CC. The anodic peak current for HQ at a working voltage of 80 mV (vs. Ag/AgCl) is related to its concentration in the 0.1 to 300 μM range (even in the presence of 0.1 mM of CC). The anodic peak current for CC at a working voltage of 184 mV is related to its concentration in the 0.5 to 400 μM range (even in the presence of 0.1 mM of HQ). The detection limits (at an S/N ratio of 3) are 24 and 71 nM for HQ and CC, respectively. The modified GCE was successfully applied to the determination of HQ and CC in aqueous solutions and gave satisfactory results.

A glassy carbon electrode was modified with gold nanoparticles, ZnS/NiS@ZnS quantum dots and L-cysteine and used for simultaneous determination of hydroquinone and catechol.

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20.
l-Dopa is the intermediate precursor of the neurotransmitter dopamine. Unlike dopamine, l-dopa easily enters the central nervous system. l-Dopa, as one of the catecholamines, is widely used as a source of dopamine in the treatment of most patients with Parkinson’s disease and epilepsy. Graphene (GR) is ideally suited for implementation in electrochemical applications due to its reported large electrical conductivity, large surface area, unique heterogeneous electron transfer rate, and low production costs. This work reports the synthesis of GR using a modified Brodie method and its application for the electrochemical determination of l-dopa in real samples. Electrochemical measurements were performed at glassy carbon electrode modified with graphene (GR/GCE) via drop casting method. Cyclic voltammograms of l-dopa at GR/GCE showed an increased current intensity compared with GCE. All the measurements were done in phosphate buffer solution 0.1 M (pH 6.2) and the oxidation peak was observed at 0.27 V vs. Ag/AgCl. The effect of scan rate showed that oxidation of l-dopa on GR/GCE was surface controlled. The oxidation peak current of l-dopa gradually increased with increasing accumulation time from 0 to 300 s and accumulation potential from 0.0 to 0.3 V and reached the maximum current response at 240 s and 0.2 V for the accumulation time and accumulation potential, respectively. Voltammetric peak currents showed a linear response for l-dopa concentration in the range of 0.04 to 79 μM and a detection limit of 0.022 μM (22 nM). The relative standard deviation for five determinations of 50 μM l-dopa was 0.52 %.  相似文献   

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