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Renewable-surface graphite–ceramic enzyme sensors for the determination of hypoxanthine in fish meat 可再生表面石墨陶瓷酶传感器测定鱼肉中的次黄嘌呤
Pub Date : 1999-01-01 DOI: 10.1039/A900896I
J. Niu, J. Lee
Sol–gel processes were used to fabricate amperometric biosensors that are active for hypoxanthine (Hx) determination. Xanthine oxidase was immobilized in the bulk of the silica–graphite matrix (SGM) to produce electrodes where new surfaces can be generated on demand by mechanical polishing. The immobilized enzyme electrodes can be used in unmediated hydrogen peroxide oxidation mode, or in unmediated and mediated oxygen reduction mode, to result in three different types of Hx biosensors with detection limits of 1.3 × 10–6, 5.6 × 10–6 and 3.8 × 10–7M, respectively. Benzyl viologen was used as the charge transfer mediator to enhance the response in the hydrogen peroxide production mode. The sensors show good linear response over a wide range of concentrations of about 1 × 10–6–1 × 10–3M. The use of bulk immobilization and the possibility of renewable surfaces have enabled the easy operation of these sensors with high stability. The experimental results from a carp sample stored under different conditions demonstrate the practicality of these sensors as simple, rapid and cost effective measurement of fish meat freshness.
采用溶胶-凝胶法制备了对次黄嘌呤(Hx)测定具有活性的安培生物传感器。黄嘌呤氧化酶被固定在硅-石墨基体(SGM)的主体中,以产生电极,在电极上可以根据需要通过机械抛光产生新的表面。固定化酶电极可以在无介导过氧化氢氧化模式下使用,也可以在无介导和有介导的氧还原模式下使用,得到三种不同类型的Hx生物传感器,检出限分别为1.3 × 10-6、5.6 × 10-6和3.8 × 10-7M。在过氧化氢生产模式下,采用紫苄基作为电荷转移介质来提高反应速度。在1 × 10-6-1 × 10-3M的浓度范围内,传感器表现出良好的线性响应。大量固定的使用和可再生表面的可能性使这些传感器具有高稳定性,易于操作。在不同条件下保存的鲤鱼样品的实验结果表明,这些传感器可以简单、快速、经济地测量鱼肉新鲜度。
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引用次数: 32
High-performance chelation ion chromatography of transition and heavy metal ions on polystyrene–divinylbenzene resin dynamically modified with 4-chlorodipicolinic acid 4-氯二吡啶酸动态改性聚苯乙烯-二乙烯苯树脂上过渡离子和重金属离子的高效螯合离子色谱
Pub Date : 1999-01-01 DOI: 10.1039/A908318I
M. J. Shaw, S. Hill, Phil Jones, P. Nesterenko
A neutral polystyrene–divinylbenzene column, combined with 4-chlorodipicolinic acid present in the mobile phase, has been developed as a chromatographic system for the high efficiency isocratic separation of transition and heavy metal ions. Retention arises from the formation of a stable dynamically coated chelating stationary phase, the capacity of which is dependent upon both the pH and ligand concentration in the eluent. The results obtained illustrate the increased loading and selectivity of this chlorinated chelating molecule in comparison with unsubstituted dipicolinic acid, exemplified by the separation of 7 metals in under 8 min. The column also displayed a strong affinity for CdII and an unusual retention for NiII, which showed a good symmetrical peak shape.
建立了一种以4-氯二吡啶酸为流动相的中性聚苯乙烯-二乙烯基苯色谱柱,作为一种高效等密度分离过渡态和重金属离子的色谱体系。保留源于稳定的动态包被螯合固定相的形成,其容量取决于洗脱液中的pH和配体浓度。结果表明,与未取代的二吡啶酸相比,氯化螯合分子的负载和选择性增加,例如在8分钟内分离了7种金属。该柱对CdII也表现出很强的亲和力,对NiII也表现出罕见的保留,并呈现出良好的对称峰形。
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引用次数: 9
FTIR spectroscopic assessment of water structure in human breast benign and malignant tissues 人乳腺良性和恶性组织中水结构的FTIR光谱评价
Pub Date : 1999-01-01 DOI: 10.1039/A905147C
Tiyu Gao, Y. Ci
Considerable compositional differences of water, nucleic acids and proteins were observed between benign and malignant breast tissues based on the curve-fitting analysis of the infrared absorption band in the frequency region 3100–3600 cm–1. Compared to normal tissue, the tendency of an increase in the proportions of strongly H-bonded water (ASBW) with biomolecules and a decrease in that of weakly H-bonded water (AWBW) was observed in abnormal tissues. Subsequently, ASBW/AWBW ratios dramatically increased. The proportions of nucleic acid–NH2 groups (ANA) and the proportions of protein N–H groups (APR) in abnormal tissues increased from those of normal tissue. The ratios ANA/APR in fibroadenoma and carcinoma tissues are higher than those in normal and hyperplasia tissues whose ANA/APR ratios are located in the same region. The ANA and ANA/APR in carcinoma tissue are the highest. These differences may be related to the cell proliferation in abnormal tissues and the unregulated growth and dedifferentiation of carcinoma cells.
通过对3100 ~ 3600 cm-1频率区域红外吸收波段的曲线拟合分析,发现乳腺良恶性组织中水分、核酸和蛋白质的组成存在较大差异。与正常组织相比,异常组织中强氢键水(ASBW)与生物分子的比例增加,弱氢键水(AWBW)的比例减少。随后,ASBW/AWBW比率急剧上升。异常组织中核酸- nh2基团(ANA)比例和蛋白N-H基团(APR)比例较正常组织增加。纤维腺瘤和癌组织中ANA/APR比值高于ANA/APR比值位于同一区域的正常组织和增生组织。ANA和ANA/APR在癌组织中最高。这些差异可能与异常组织中的细胞增殖和癌细胞的不调节生长和去分化有关。
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引用次数: 4
Preliminary study on fluorimetric detection of aflatoxins Q1, P1 and B1 using heptakis-di-O-methyl-β-cyclodextrin as post-column HPLC reagent 柱后高效液相色谱法检测黄曲霉毒素Q1、P1和B1的初步研究
Pub Date : 1999-01-01 DOI: 10.1039/A809150A
B. Vázquez, C. Fente, C. Franco, A. Cepeda, G. Mahuzier, P. Prognon
Post-column fluorimetric detection for the determination of aflatoxins Q1, P1 and B1 was carried out by using HPLC with a 2.0 mm id column. The post-column reagent consisted of a 10–2M aqueous solution of heptakis-di-O-methyl-β-cyclodextrin. The fluorescence enhancement achieved was 37- and 27-fold for AFQ1 and AFB1, respectively, whereas the AFP1 signal was increased just about 2-fold. With the proposed method, aflatoxins Q1, P1 and B1 can be simultaneously determined in human urine. The detection limits (S/N = 3) were as follows: 0.7 ng ml–1 for AFQ1, 0.5 ng ml–1 for AFP1 and 0.3 ng ml–1 for AFB1.
柱后荧光法测定黄曲霉毒素Q1、P1和B1,色谱柱为2.0 mm。柱后试剂为10-2M的庚-二o -甲基-β-环糊精水溶液。AFQ1和AFB1的荧光增强分别为37倍和27倍,而AFP1信号仅增加约2倍。该方法可同时测定人体尿液中的黄曲霉毒素Q1、P1和B1。检出限(S/N = 3)为:AFQ1为0.7 ng ml-1, AFP1为0.5 ng ml-1, AFB1为0.3 ng ml-1。
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引用次数: 19
Ceramic microchips for capillary electrophoresis–electrochemistry 毛细管电泳-电化学用陶瓷微芯片
Pub Date : 1999-01-01 DOI: 10.1039/A904807C
C. Henry, M. Zhong, S. Lunte, Moon Kim, H. Bau, J. Santiago
A capillary electrophoresis–electrochemistry chip constructed from low-temperature co-fired ceramic (LTCC) tape is presented. This is the first report of such a chip constructed in this manner using these materials. Electroosmotic flow at pH 7 is demonstrated by the migration of a neutral marker, catechol. The separation and detection of two phenolic compounds are presented.
介绍了一种由低温共烧陶瓷(LTCC)带构成的毛细管电泳-电化学芯片。这是使用这些材料以这种方式构建这样一个芯片的第一个报告。pH值为7的电渗透流动通过中性标记物儿茶酚的迁移来证明。介绍了两种酚类化合物的分离和检测方法。
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引用次数: 53
Liquid chromatography–mass spectrometric analysis of phenylurea herbicides and their degradation products using an atmospheric pressure ionization interface 常压电离界面液相色谱-质谱法分析苯脲类除草剂及其降解产物
Pub Date : 1998-01-01 DOI: 10.1039/A709147H
T. Yarita, K. Sugino, T. Ihara, A. Nomura
A method was developed for the determination of two phenylurea herbicides and their degradation products using liquid chromatography–atmospheric pressure chemical ionization (APCI)-mass spectrometry without any additives in the mobile phase. The APCI detection sensitivity of these compounds was maximized when the vaporizer temperature was set at 250 °C and a positive-ion detection mode was chosen. Under these conditions, the detection limits (S/N = 3) of these compounds in total-ion and selected-ion monitoring were 2.5–3.0 and 0.12–0.26 ng, respectively. In a biodegradability test on diuron, small quantities of degradation products could be determined by the proposed method.
建立了流动相不添加添加剂的液相色谱-常压化学电离(APCI)-质谱联用法测定两种苯脲类除草剂及其降解产物的方法。当汽化器温度为250℃,选择正离子检测模式时,APCI检测灵敏度最大。在此条件下,总离子监测和选择离子监测的检出限(S/N = 3)分别为2.5 ~ 3.0 ng和0.12 ~ 0.26 ng。在diuron的生物降解性测试中,可以通过所提出的方法确定少量降解产物。
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引用次数: 5
Self-assembled silanes and the thiol functionalization of surfaces 自组装硅烷和表面的硫醇功能化
Pub Date : 1998-01-01 DOI: 10.1039/A807021K
M. McGovern, M. Thompson
The relative thickness and coverage of the silanes, mercaptopropyltrimethoxysilane and 1-(trifluoroacetato-)-11-trichlorosilyl-undecane subsequent to reaction on silicon surfaces has been assessed by X-ray photoelectron spectroscopic analysis. Use of the probe, N-pentafluorophenyl-N′-iodoacetyl hydrazide, allows an estimation of the availability of thiol groups on the substrate surface following reaction in air and in O2-free conditions. Although the trimethoxysilane generates multilayer structures, it is only capable of attaching 3.5 times less probe than the fluorine-containing silane. The results of these experiments confirm that 1-(trifluoroacetato-)-11-trichlorosilyl-undecane is a much more effective linking agent for the immobilization of biomolecules to substrate surfaces.
用x射线光电子能谱分析评价了硅烷、巯基丙基三甲氧基硅烷和1-(三氟乙酸-)-11-三氯硅十一烷在硅表面反应后的相对厚度和覆盖范围。使用探针n -五氟苯基- n ' -碘乙酰肼,可以估计在空气和无o2条件下反应后底物表面巯基的可用性。虽然三甲氧基硅烷可以产生多层结构,但其附着探针的数量仅为含氟硅烷的3.5倍。这些实验结果证实,1-(三氟乙酸-)-11-三氯硅十一烷是一种更有效的连接剂,用于固定化生物分子到底物表面。
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引用次数: 10
On-flow identification of metabolites of paracetamol from human urine using directly coupled CZE–NMR and CEC–NMR spectroscopy 用直接耦合cce - nmr和CEC-NMR谱分析人尿中扑热息痛代谢物的流动鉴定
Pub Date : 1998-01-01 DOI: 10.1039/A803671C
K. Pusecker, J. Schewitz, P. Gfrörer, L. Tseng, K. Albert, E. Bayer, I. Wilson, N. J. Bailey, G. Scarfe, J. Nicholson, J. Lindon
Direct NMR spectroscopic detection on-flow to capillary electrophoresis (CE) or capillary electrochromatography (CEC) was applied to the separation of metabolites of paracetamol from an extract of human urine. The detection and characterisation of the major metabolites, the glucuronide and sulfate conjugates of the drug as well as identification of the endogenous material hippurate was achieved. This demonstrates that NMR detection and identification of drug metabolites is possible with nanolitre volumes of analyte.
采用毛细管电泳(CE)或毛细管电色谱(CEC)直接核磁共振波谱法对人尿提取物中扑热息痛的代谢物进行分离。实现了主要代谢物、葡萄糖醛酸盐和硫酸盐缀合物的检测和表征,以及内源性物质马嘌呤的鉴定。这表明,核磁共振检测和鉴定药物代谢物是可能的与纳升体积的分析物。
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引用次数: 38
Behaviour of selenium compounds in FI-HG-AAS 硒化合物在FI-HG-AAS中的行为
Pub Date : 1998-01-01 DOI: 10.1039/A805575K
A. Chatterjee, K. Irgolic
The borohydride active volatile compound formation potential of twelve selenium compounds [selenous acid, selenic acid, selenocystine (Secys), selenohomocystine (Sehcys), selenomethionine (Semet), selenoethionine (Seet), trimethylselenonium iodide (TmSe), selenocystathionine (Secystha), selenocystamine (Secysta), selenourea (Seur), selenocholine (Sech), and dimethyl(3-amino-3- carboxy-1-propyl)selenonium iodide (DmpSe)] were investigated in a FI-HG system with different sodium borohydride concentrations (0.3% in 0.1% sodium hydroxide, and 0.5, 0.7, and 1.0% in 0.2% sodium hydroxide) in the presence of 3 M hydrochloric acid using an atomic absorption spectrometer as selenium-specific detector. Percentage recoveries with respect to selenous acid of selenic acid, Secys, Sehcys, Semet, Seet, TmSe, Secystha; Secysta, Seur, Sech, and DmpSe were 0, 10.3, 19.7, 23.5, 32.4, 13.7, 16.5, 16.5, 11.3, 5.6 and 7.7%, respectively in the presence of 0.3% borohydride stabilized with 0.1% sodium hydroxide. By multiplying the borohydride concentrations, percentage recoveries of TmSe, DmpSe, Sech, Sehcys and Secysta were elevated, whereas those of Semet, Seet and Seur were reduced. However, percentage recoveries of Secys and Secystha remained almost uniform within the entire borohydride range. TmSe exhibited a 105% recovery with respect to selenous acid at 1.0% borohydride concentration, whereas selenic acid was inert to borohydride active volatile compound formation.
硒酸、硒酸、硒半胱氨酸(Secys)、硒同半胱氨酸(Sehcys)、硒代蛋氨酸(Semet)、硒代蛋氨酸(Seet)、硒代蛋氨酸(Seet)、三甲基硒碘化铵(TmSe)、硒半胱氨酸(Secystha)、硒半胺(Secysta)、硒脲(Seur)、硒胆碱(Sech)、在不同硼氢化钠浓度(0.1%氢氧化钠浓度为0.3%,0.2%氢氧化钠浓度为0.5、0.7和1.0%)的FI-HG体系中,在3 M盐酸存在下,利用原子吸收光谱仪作为硒特异性检测器,研究了二甲基(3-氨基-3-羧基-1-丙基)碘化硒(DmpSe)。selenic acid、Secys、Sehcys、Semet、Seet、TmSe、Secystha中亚硒酸的回收率;在0.3%硼氢化物和0.1%氢氧化钠稳定作用下,Secysta、Seur、Sech和DmpSe分别为0、10.3、19.7、23.5、32.4、13.7、16.5、16.5、11.3、5.6和7.7%。通过增加硼氢化物浓度,提高了TmSe、DmpSe、Sech、Sehcys和Secysta的回收率,降低了Semet、Seet和Seur的回收率。然而,在整个硼氢化物范围内,Secys和Secystha的回收率几乎保持一致。当硼氢化物浓度为1.0%时,TmSe对亚硒酸的回收率为105%,而亚硒酸对硼氢化物活性挥发性化合物的形成是惰性的。
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引用次数: 18
Comparison of three different microemulsion systems as the run buffer for the capillary electrophoretic separation of ketone test solutes 三种不同微乳液体系作为毛细管电泳分离酮类测试溶质的缓冲液的比较
Pub Date : 1998-01-01 DOI: 10.1039/A804998J
H. Watarai, I. Takahashi
Capillary electrophoretic behavior of ketones and β-diketones was examined using anionic, nonionic and cationic oil in water (o/w) microemulsions as separation media, containing naphthalene as a fluorophore for means of indirect fluorescence detection. The migration behavior was greatly dependent on the charge type of microemulsions as well as on the composition and pH. Among the systems examined, sodium dodecyl sulfate (SDS) microemulsions were the most advantageous because of the wider separation window, the higher dissolution capacity and the rapid distribution rate. Capacity factors of the solutes in the electrophoresis employing SDS microemulsions were correlated to the distribution and interfacial adsorption parameters determined in bulk two-phase systems.
以阴离子、非离子和阳离子油水溶液(0 /w)为分离介质,以萘为荧光基团间接荧光检测,研究了酮类和β-二酮类的毛细管电泳行为。迁移行为在很大程度上取决于微乳液的电荷类型、组成和ph值。在所研究的体系中,十二烷基硫酸钠(SDS)微乳液因其更宽的分离窗口、更高的溶解能力和更快的分布速率而最具优势。SDS微乳电泳中溶质的容量因子与其在两相体系中的分布和界面吸附参数相关。
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引用次数: 12
期刊
Analytical Communications
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