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Vaclav Diopan Violetta Shestivska Ondrej Zitka Michaela Galiova Vojtech Adam Jozef Kaiser Ales Horna Karel Novotny Miroslav Liska Ladislav Havel Josef Zehnalek Rene Kizek 《Electroanalysis》2010,22(11):1248-1259
The main aim of this paper is to utilize high performance liquid chromatography with electrochemical detection for determination of thiols content in plants tissues of lettuce treated with lead(II) ions (0, 0.5 and 1 mM). We used two HPLC‐ED instruments: HPLC coupled with one channel amperometric detector and HPLC coupled with twelve channel coulometric detector to detect simultaneously twelve thiols. The detection limits of thiols measured by CoulArray detector were about two magnitudes lower in comparison to those measured by Coulochem III detector and were from tens to hundreds pM. Under the optimal conditions, we utilized HPLC‐CoulArray detector for analysis of tissues from lettuce plants. In addition, distribution and accumulation of lead ions with high spatial resolution was monitored using laser induced breakdown spectroscopy. 相似文献
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液相色谱-脉冲安培电化学法测定硫酸卡那霉素中各组分含量 总被引:1,自引:0,他引:1
建立了一种用反相离子对液相色谱(LC)分离,以金电极为工作电极的脉冲安培电化学法(PAD)直接检测硫酸卡那霉素中主要组分及杂质含量的分析方法。流动相为0.033mol/L草酸、0.012mol/L七氟丁酸、105mL/L乙腈,用稀NaOH调节pH至3.4。考察了各色谱参数对分离测定的影响。实验证明,本方法不需要衍生化,可直接检测硫酸卡那霉素。与报道的其它方法相比,本方法不仅能使硫酸卡那霉素中的卡那霉素A、B得到了很好的分离,还分离出了其它一些未能确证的组分。如用质谱法等对未知组分进行确证后,对硫酸卡那霉素原料药、注射液、滴眼液及兽药等实际样品中的卡那霉素各组分进行测定。可望成为一种标准分析方法。 相似文献
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Liquid chromatography with pulsed amperometric detection (PAD) at an Au electrode was successfully applied for speciation of mercury: inorganic mercury, methylmercury and ethylmercury. The optimized conditions for triple-step potential waveforms utilized in PAD were: E1 1800 mV, t1 50 ms; E2 300 mV, t2 3850 ms; E3 750 mV, t3 100 ms; mercury oxidation was monitored at E3. With the eluent of HClO4 (0.10 M) + KCl (1.0 mM) + CH3CN (1.0%) at a flow rate 0.80 mL/min, three mercury species were fully separated in 6 min on a glass column (3 mm × 10 cm) packed with Chemcosorb C18 (5 μm). However, the first peak (inorganic mercury) was commonly overlapped by the solvent front. The relative standard deviations (n = 6) for methylmercury (15 ppb) and ethylmercury (30 ppb) were 4.2% and 2.8%, respectively. The linear range tested was 2 – 500 ppb (r = 0.9998) for methylmercury, and was 4 – 1000 ppb (r = 1.000) for ethylmercury. The detection limits (S/N = 3) were 1.2 ppb and 1.8 ppb for methylmercury and ethylmercury, respectively. The results of determination of the mercury-containing species thimerosat in three commercial contact-lens solutions agreed satisfactorily with the expected values. 相似文献
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Commercial Screen‐Printed Gold Electrodes for the Detection and Quantification of Aminothiols in Human Plasma by Liquid Chromatography with Electrochemical Detection 下载免费PDF全文
Santiago Cavanillas Núria Serrano José Manuel Díaz‐Cruz Cristina Ariño Miquel Esteban 《Electroanalysis》2014,26(3):581-587
In order to show the possibilities of screen‐printed electrodes in HPLC detection, a method is presented for routine quantification of aminothiols in human plasma. It uses commercial gold screen‐printed electrodes and provides a rapid, simple and economical procedure with a disposable detector and without any additional electrode. By working at 98 : 2 (0.05 % trifluoroacetic acid: methanol) and 0.9 V, it allows us to determine cysteine (Cys), cysteinyl‐glycine (Cys‐Gly), and homocysteine (HCys) at μmol/L levels. The method was validated, and linearity range, detection and quantification limits, precision and accuracy were evaluated by external calibration and by using N‐acetylcysteine as internal standard, which exhibited better precision. 相似文献
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建立了一种新的用反相离子对液相色谱(LC)分离,以金电极为工作电极的脉冲安培电化学法(PAD)直接检测硫酸庆大霉素中各组分含量的分析方法。流动相为0.033 mol/L草酸、0.012 mol/L七氟丁酸、210 mL/L乙睛,用稀NaOH调节pH至3.4。与报道的其它方法相比,该方法能使庆大霉素各有效组分C1、C1 a、C2、C2 a很好分离,整个分析过程<30 m in。考察了各色谱参数对分离测定的影响。实验证明,本方法不需要衍生化,可直接检测硫酸庆大霉素。 相似文献
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液相色谱电化学检测抗结核药物—异烟肼 总被引:3,自引:0,他引:3
本文讨论了以无有机溶剂存在的水溶液为流动相异烟肼的液相色谱一薄层安培检测法。在所选定的实验条件下,检测限达2ng。应用本法分析了片剂中异烟肼的含量 相似文献
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Determination of Aldehydes and Ketones in Fuel Ethanol by High-Performance Liquid Chromatography with Electrochemical Detection 总被引:1,自引:0,他引:1
A. A. Saczk L. L. Okumura M. F. de Oliveira M. V. B. Zanoni N. R. Stradiotto 《Chromatographia》2006,63(1-2):45-51
A new methodology was developed for analysis of aldehydes and ketones in fuel ethanol by high-performance liquid chromatography
(HPLC) coupled to electrochemical detection. The electrochemical oxidation of 5-hydroxymethylfurfural, 2-furfuraldehyde, butyraldehyde,
acetone and methyl ethyl ketone derivatized with 2,4-dinitrophenylhydrazine (DNPH) at glassy carbon electrode present a well
defined wave at +0.94 V; +0.99 V; +1.29 V; +1.15 V and +1.18 V, respectively which are the basis for its determination on
electrochemical detector. The carbonyl compounds derivatized were separated by a reverse-phase column under isocratic conditions
with a mobile phase containing a binary mixture of methanol / LiClO4(aq) at a concentration of 1.0 × 10−3 mol L−1 (80:20 v/v) and a flow-rate of 1.1mL min−1 . The optimum potential for the electrochemical detection of aldehydes-DNPH and ketones-DNPH was +1.0 V vs. Ag/AgCl. The
analytical curve of aldehydes-DNPH and ketones-DNPH presented linearity over the range 5.0 to 400.0 ng mL−1, with detection limits of 1.7 to 2.0 ng mL−1 and quantification limits from 5.0 to 6.2 ng mL−1, using injection volume of 20 μL. The proposed methodology was simple, low time-consuming (15 min/analysis) and presented
analytical recovery higher than 95%. 相似文献
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《Analytical letters》2012,45(5):786-792
Citrinin is a toxic product of secondary metabolism of fungi, such as certain Aspergillus, Penicillium, and Monascus species that are usually contaminating cereals. A new sensitive liquid chromatographic method with fluorescence detection was developed, validated, and applied for citrinin determination. The method is based on reversed-phase separation at pH 2.5, where citrinin exhibits the highest fluorescence quantum yield. In this setup, no derivatization step is needed. The method shows linearity in the range between 0.2 μg/mL and 0.1 mg/mL. The detection limit reached is 90 ng/mL (3.6 × 10?7 M). Validated method was successfully applied on analysis of spiked and real cereal samples. 相似文献
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多通道电化学检测是按照新一代电化学检测仪器的要求而设计的产品。它具有使用方便,快速准确,排除干扰等多种功能,非常适用于复杂体系中化合物的测定。本文报道了液相色谱/四通道电化学检测法在天然酚类化合物测定中的应用。此方法能快速获得待测物的流体动力学伏安图(HDV图);色谱峰的鉴定可靠;在不同电压下同时定量测定不同的化合物。本文以测定蜂蜜中的酚酸类化合物及绿茶中的儿茶素类化合物为例对此分析方法进行了阐述。 相似文献
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《Analytical letters》2012,45(12):2565-2573
Abstract The electrochemical behaviour of vitamin D3 and 25-hydroxyvitamin D3 (25-OH D3) in a high performance liquid chromatography system using amperometric detection is described. Separation is carried out using a C18 reversed-phase column and the optimum mobile phase was a 0.1 M LiClO4 solution in methanol-water (97:3, v/v) at a flow rate of 1.25 ml/min. 25-OH D3 and vitamin D3 were eluted with good resolution at retention times of 3 and 6 minutes respectively, and determined by amperometric detection with a glassy carbon electrode at + 1.050 V (vs Ag/AgCl). Calibration graphs for both substances showed good linearity when amounts of vitamin D3 between 18 and 312 ng and 27 and 412 ng of 25-OH D3 were injected. Detection limits of 8 ng (vitamin D3) and 25 ng (25-OH D3); relative standard deviations of 3.2% (vitamin D3) and 5.8% (25-OH D3) were obtained. 相似文献
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Three synthetic phenolic antioxidants, tertiary butyl hydroquinone, butylated hydroxytoluene, and butylated hydroxyanisole, were determined in vegetable oil and oil-enriched food by high-performance liquid chromatography (HPLC) with electrochemical detection. The separation was achieved using a reverse-phase column and gradient elution with methanol and 1% acetic acid. The limits of detection and quantification of the analytes were 2–120 lower, higher than those obtained by diode-array detection. The recoveries were 103.3% for tertiary butyl hydroquinone, 97.3% for butylated hydroxyanisole, and 95.2% for butylated hydroxytoluene. The results showed that HPLC with electrochemical detection is suitable for the quantification of low concentrations of phenolic antioxidants in vegetable oil and oil-enriched food with high sensitivity and accuracy. 相似文献
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采用固相萃取技术,结合超高效液相色谱-荧光分析(UPLC-FLD)手段,建立了人体尿液中酪氨酸、对羟苯基乳酸和对羟苯基乙酸的同时测定新方法。系统探讨了不同机理下,应用固相萃取技术处理尿液的效果,最终选用Clean-Screen DAU混合固相萃取小柱处理尿液,成功地除去了大量干扰物质。在优化的实验条件下,上述三种化合物线性关系良好(R20.9996),检测限均为0.016mg/L。健康人和癌症病人尿液三个添加水平的平均回收率在86.9%~107.9%之间,相对标准偏差(RSD)小于2.8%。该方法快速、灵敏度高、选择性好,可用于人体尿液中三组分的同时测定。 相似文献
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离子色谱中的安培检测方法及其应用 总被引:1,自引:0,他引:1
介绍了离子色谱中的安培检测方法(包括恒电位安培检测法、脉冲安培检测法和积分脉冲安培检测法)的原理和应用。脉冲安培检测法与高效阴离子交换色谱结合(HPAEC-PAD)是一种新的分析糖类化合物的方法;积分脉冲安培检测法与高效阴离子交换色谱结合(HPAEC-IPAD)是一种新的氨基酸分析方法。 相似文献
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