苏丹红Ⅰ号的毛细管电泳安培检测

建立了毛细管电泳安培法测定苏丹红Ⅰ号的方法.考察了缓冲液种类、浓度和pH值,分离电压、进样时间、检测电位等因素对分离检测的影响.以10 mmol/L硼砂盐(pH 9.3)为缓冲液,检测电位1.05 V(vs.SCE),分离电压21 kV,电动进样(12 kV)8 s,苏丹红Ⅰ号在1.13×10-9～1.13×10-7mol/L范围内,浓度与峰面积具有良好的线性关系,回收率为93.5%～102.7 %,检测限为1.13×10-9 mol/L.该方法成功应用于辣椒粉样品的检测,结果令人满意.     

Determination of carbohydrates by capillary zone electrophoresis with amperometric detection at a nano-nickel oxide modified carbon paste electrode

In this paper, a nano-NiO modified carbon paste electrode in capillary zone electrophoresis with amperometric detection (CZE-AD) was firstly applied to the determination of carbohydrates. Effects of several important factors such as detection potential, the concentration of running buffer, separation voltage and injection time were investigated to acquire the optimum conditions. Under the selected optimum conditions, three carbohydrates: glucose, sucrose and fructose could be perfectly separated within 20 min. The relationships between peak current and concentration of three carbohydrates were linear over about 3 orders of magnitude with detection limits (S/N = 3) ranging from 3.0 × 10⁻⁷ to 6.0 × 10⁻⁷ mol L⁻¹. The electrode was stable, and can be used for at least one week. The proposed method has been successfully applied to monitor carbohydrates in the real samples with satisfactory assay results.     

Study on extraction efficiency of natural antioxidant in coffee by capillary electrophoresis with amperometric detection

Capillary electrophoresis with amperometric detection (CE-AD) has been used for the determination of catechin, rutin, ferulic acid, o-dihydroxybenzene, chlorogenic acid, caffeic acid, gallic acid, and protocatechuic acid in coffee. Comparison of extraction efficiency of antioxidants using different polar solvents was also conducted by this method. Effects of several important factors including the acidity and concentration of running buffer, separation voltage, and working electrode potential, were evaluated to obtain the optimum analysis conditions. The working electrode was a 300 um carbon disc electrode at an applied potential of +0.95 V (vs. saturated calomel reference electrode). Under the optimum conditions, the analytes can be well separated within 26 min in a 75 cm length fused-silica capillary (i.d. 2.5 × 10⁻⁵ m). The current response was linear over three orders of magnitude with detection limits (S/N = 3) ranging from 6.0 × 10⁻⁸ to 3.6 × 10⁻⁷ g/mL for all analytes.     

高效毛细管区带电泳-间接紫外法测定食品中三氯蔗糖

目的建立利用毛细管区带电泳-间接紫外法测定食品中三氯蔗糖的方法。方法样品用超纯水提取,离心所得的上清液直接进样,以未涂层熔融石英毛细管(50μm×60.2 cm)为分离柱,3 mmol/L 3,5-二硝基苯甲酸+10 mmol/L磷酸钠+12 mmol/L氢氧化钠(p H=12.58)+0.5 mmol/L十六烷基三甲基溴化铵为分离缓冲液;检测波长200 nm,分离电压-20 k V。采用校正峰面积外标法进行定量。结果方法检出限为10 mg/L,定量限为30 mg/L,线性范围为30~300 mg/L,线性相关系数r=0.999 1。低、中、高3个质量浓度(40、60及80 mg/L)的加标回收率分别为108.1%、102.6%、103.5%,相对标准偏差(RSD)分别为1.3%、1.3%及1.0%,方法精密度为2.0%。结论本研究样品前处理操作简单,20 min之内即可完成三氯蔗糖的含量分析(预清洗6 min,分离13 min),实现了与其结构相似但又同时存在于食品中蔗糖的分离,且试剂及样品消耗量少,适用于实验室对于食品中三氯蔗糖的检测。     

毛细管区带电泳-间接紫外测定食品中木糖醇

目的建立毛细管区带电泳间接紫外测定食品中木糖醇的新方法。方法样品用超纯水提取后离心,过0.45μm膜后上机进样。以未涂敷熔融石英毛细管(50μm×60.2 cm)为毛细管分离柱,以8 mmol/L 3,5-二硝基苯甲酸、10 mmol/L硼砂和0.5 mmol/L十六烷基三甲基溴化铵为分离缓冲溶液。分离电压为-20 k V,检测波长为200 nm,用外标法定量。结果方法检出限为3.00 mg/L(S/N=3),定量限为10.00 mg/L(S/N=9),线性范围为10.00~300.0 mg/L,线性相关系数r为0.9994。在20.00、40.00、80.00 mg/L添加水平下,平均回收率分别为103.2%、103.3%及104.8%,相对标准偏差分别为0.5%、1.2%及0.7%(n=3)。结论该方法简单快速,11 min内即可完成一次样品分析(清洗6 min、分离5 min),试剂及样品消耗量少,适用于食品中木糖醇的检测。     

毛细管区带电泳-间接紫外检测法测定婴儿配方奶粉中的胆碱

目的建立毛细管区带电泳-间接紫外检测法测定婴儿配方奶粉中胆碱含量的新方法。方法用5 mmol/L乙酸提取婴儿配方奶粉样品中的胆碱,涡旋混匀、9000 r/min离心,上清液经0.45μm醋酸纤维素滤膜过滤后进样。用未涂覆熔融石英毛细管75μm×70 cm(有效长度:60 cm)作为分离柱。以10 mmol/L磷酸二氢钠+20 mmol/L磷酸+7 mmol/L 4-甲基咪唑为分离缓冲体系。分离电压为28 k V,进样压力及时间为0.5 psi、10 s,检测波长为214 nm。结果胆碱的校正峰面积与质量浓度在8.7~86.8 mg/L范围内间线性关系良好,相关系数为0.9997、检出限为2.6 mg/L、定量限为8.7 mg/L,方法的日内和日间精密度分别为1.9%和3.9%(n=7)。3个质量浓度添加水平的平均加标回收率分别为98.8%、95.2%及97.6%,相应RSD分别为0.8%、0.9%及0.6%(n=5)。用本法分析了10件婴儿配方奶粉样品,均获满意结果。结论本方法简单、无需有机溶剂,适用于婴儿配方奶粉中胆碱的常规检测。     

Simple determination of main organic acids in grape juice and wine by using capillary zone electrophoresis with direct UV detection

An accurate, simple and rapid capillary zone electrophoresis (CZE) method with direct UV detection has been set up for the determination of main organic acids in grape juice and wine. The determination of tartaric, malic, and citric acids in grape juices and tartaric, malic, succinic, acetic, lactic and citric acids in wines can be achieved in less than 3 min with only a simple dilution and filtration treatment of the sample. Validation parameters of the method as detection and quantification limits, linearity, precision (intraday and interday analysis) and recovery were also studied in grape juice, white wine, rose wine and red wine, separately. The proposed method decreases the analysis times of the previous reported CZE methods and allows the rapid control of the grape maturity, the winemaking processes and the detection of wine alterations and/or illnesses.     

Rapid determination of sodium in milk and milk products by capillary zone electrophoresis

A capillary zone electrophoresis method for the determination of Na in milk and milk products was developed and compared with an International Organization for Standardization/International Dairy Federation standard method that is based on flame atomic absorption spectrometry. The adoption of a background electrolyte consisting of 10 mM imidazole adjusted to pH 3.75 by the addition of oxalic acid allowed baseline separation of Na from other milk cations and from Li ion, which was adopted as an internal standard. Method validation was performed and the results for linearity, precision, limit of detection, limit of quantification, and recovery are presented. The procedure was tested on commercial milk samples differing in fat content (whole, semiskimmed, and skimmed) and processing conditions (pasteurization, UHT sterilization, and microfiltration). The reliability of the method was confirmed for different varieties of cheese and other milk products. The method enables the routine measurement of Na content by a rapid and accurate capillary zone electrophoresis procedure.     

毛细管区带电泳非衍生化直接测定蜂蜜中糖含量

建立了一种新的测定蜂蜜中糖含量的方法,并探讨了检测机理。以弹性石英毛细管柱（有效长度/总长度=52/62 cm）为分离柱,130 mmol/L的Na OH+30 mmol/L的Na2HPO4溶液（p H=12.8）为运行缓冲液,温度20℃,分离电压在1 min内升至16 k V,测定波长为270 nm,以20 psi的压力进样,内标峰面积法计算含量。经测定:蜂蜜样品中果糖、葡萄糖、蔗糖和麦芽糖含量分别为42.8%、36.1%、4.67%和2.16%,检测机理可能是糖在强碱溶液中发生光化学反应,检测在非平衡态进行;果糖、葡萄糖在0.04⁰.8 mg/m L,蔗糖、麦芽糖在0.005⁰.1 mg/m L范围内线性关系良好;最低检测限果糖和葡萄糖为9μg/m L,蔗糖和麦芽糖为18μg/m L,明显低于高效液相色谱示差检测法;果糖、葡萄糖、蔗糖、麦芽糖回收率分别为99.4%、97.9%、97.1%、102.7%,方法回收率良好。此方法准确、简便,可用于蜂蜜中糖的测定。      

Determination of levoglucosan from smoke samples using microchip capillary electrophoresis with pulsed amperometric detection

Separation and detection of native anhydrous carbohydrates derived from the combustion of biomass using an electrophoretic microchip with pulsed amperometric detection (PAD) is described. Levoglucosan represents the largest single component of the water extractable organics in smoke particles and can be used to trace forest fires or discriminate urban air pollution sources. Detection of levoglucosan and other sugar anhydrides in both source and ambient aerosol samples is typically performed by gas chromatographic (GC) separation with mass spectrometric (MS) detection. This method is cost, time, and labor intensive, typically involving a multistep solvent extraction, chemical derivatization, and finally analysis by GC/MS. However, it provides a rich wealth of chemical information as the result of the combination of a separation method and MS and exhibits good sensitivity. In contrast, microchip capillary electrophoresis offers the possibility of performing simpler, less expensive, and faster analysis. In addition, integrated devices can be fabricated and incorporated with an aerosol collection system to perform semicontinuous, onsite analysis. In the present report, the effect of the separation potential, buffer pH and composition, injection time, and pulsed amperometric detection parameters were studied in an effort to optimize both the separation and detection of anhydrous sugars. Using the optimized conditions, the analysis can be performed in less than a minute, with detection limits ranging from 22 fmol (16.7 microM) for levoglucosan to 336 fmol (258.7 microM) for galactosan. To demonstrate the capabilities of the device, a comparison was made between GC/MS and microchip electrophoresis using an aerosol source sample generated in a wood-burning chamber. A second example utilizing an ambient aerosol sample illustrates a matrix interference necessitating additional method development for application to samples not dominated by wood smoke.     

毛细管区带电泳-间接紫外检测法测定饮用水中5种阴离子

目的建立毛细管区带电泳-间接紫外检测法测定饮用水中5种阴离子的新方法。方法样品无需滤膜过滤可直接进样。用未涂覆熔融石英毛细管(75μm×80 cm,有效长度为70 cm)作为分离柱。以20 mmol/L邻苯二甲酸、100 mmol/L二乙醇胺和0.5 mmol/L十六烷基三甲基溴化铵为分离缓冲体系。结果 Cl~-、NO_3~-、SO_4~(2-)、F~-和H_2PO_4~-这5种阴离子的校正峰面积与质量浓度分别在0.5～100.0、0.2～20.0、0.5～100.0、0.2～4.0和0.2～5.0 mg/L范围内呈线性相关,相关系数分别为0.998 8、0.999 9、0.999 7、0.999 7、0.999 8。检出限均为0.05 mg/L,定量限均为0.15 mg/L,方法精密度均小于5%(n=6)。低、中和高质量浓度加标回收率在81.6%～108.6%之间,相对标准偏差在0.6%～3.7%之间(n=6)。用本法分析了7份饮用水样品,并与离子色谱法的结果相比较,除矿泉水中Cl~-结果偏低外,其余基本吻合。结论本方法简单,所用试剂环保,为饮用水中5种阴离子的常规检测提供了一种新方法,但不适合测定水样中低浓度的Cl~-。     

毛细管电泳电化学发光法快速分离检测水果中的精胺

目的:建立水果中精胺含量测定的毛细管电泳电化学发光(CE-ECL)法。方法:利用CE-ECL技术建立了一种高效快速准确的测定水果中精胺含量的的方法。结果:精胺标准溶液在2×10^-4~3×10^-1 mmol/L浓度范围内与ECL强度呈良好的线性关系,其线性方程为I=1114.2c+99.41,相关系数r=0.9996(n=5),检出限(S/N=3)为9.9×10^-5 mmol/L,加标回收率分别为95.1%~101.2%、99.0%~100.8%和100.6%~106.0%。结论:该方法简单、准确,重复性好,可用于研究果蔬采后保鲜贮藏和延长货架期。     

Multi‐residue analysis of sulfonamides in animal tissues by capillary zone electrophoresis with electrochemical detection

BACKGROUND: The objective of this study was to adapt and improve previously published analysis methods aimed at the simultaneous determination of sulfonamide residues in edible animal tissues by capillary zone electrophoresis with electrochemical detection. RESULTS: The effects of several factors such as the acidity and concentration of running buffer, the separation voltage, the applied potential and the injection time on CZE‐ED were investigated. Complete separation of six sulfonamides was achieved within 17 min by using 40 mmol L^?1 Na₂B₄O₇/25 mmol L^?1 KH₂PO₄ (pH 6.2) at an applied voltage of 18 kV. Excellent linearity was obtained over two orders of magnitude with the improved detection limits (S/N = 3) ranged from 1.7 × 10^?7 to 4.4 × 10^?9 g mL^?1 for all six sulfonamides in comparison with previous reports. A solvent extraction/centrifuge/evaporation procedure was used to extract sulfonamides from animal tissues, sample clean‐up and pre‐concentration of sulfonamides prior to CZE‐ED analysis. Good recoveries from 81% to 92% were achieved. CONCLUSION: Results obtained in this work indicated that the proposed CZE‐ED method was sensitive, rapid and simple for the simultaneous determination of sulfonamides in edible animal tissues. Therefore, the new faster and easy handling procedure provides an additional powerful tool that can be employed for the analysis of sulfonamide residues in foodstuff. Copyright © 2009 Society of Chemical Industry     

高效毛细管电泳-紫外检测法分离测定氨基酸的含量

利用高效毛细管区带电泳直接紫外检测法对8种非衍生化氨基酸进行了分离分析条件的研究,采用重力进样,进样高度20cm,进样时间30s,弹性石英毛细管内径75μm,有效分离长度48cm,分离电压-20kv,在浓度为50mmol/L,pH10的硼砂缓冲溶液中加入0.5mmol/L的十六烷基三甲基溴化铵作为电渗流改性剂,在4min内,8种氨基酸得到了有效分离。各氨基酸的线性范围为5～150μg/mL或1～80μg/mL,检出限在0.5～2μg/mL之间。应用于由糖蜜生产亮氨酸的发酵液中缬氨酸和亮氨酸含量的测定,结果满意。     

Simultaneous analysis of acidulants and preservatives in food samples by using capillary zone electrophoresis with indirect UV detection

Capillary zone electrophoresis with indirect UV detection was developed for the simultaneous analysis of acidulants and preservatives in food samples. When a solution of tris (hydroxymethyl) aminomethane, trimellitic acid and poly (vinyl alcohol) was used as the background electrolyte, the nine acidulants and four preservatives listed in the Japanese Food Sanitation Law were detected within 8 min. The calibration curves plotted from the peak height of each analyte were linear with a correlation coefficient of 0.99. The relative standard deviations (n = 10) of the peak height ranged from 1.2% to 4.7%. The detection limits for these species ranged from 0.6 to 5.3 mg/L at a signal-to-noise ratio of three. The method developed method was applied to the simultaneous analysis of acidulants and preservatives in a wide variety of food samples.     

A rapid quantitative determination of phenolic acids in Brassica oleracea by capillary zone electrophoresis

A simple and rapid capillary zone electrophoresis method to quantitatively determine the phenolic acid contents in brassica vegetables is described. Phenolic compounds were extracted from broccoli, broccolini, Brussels sprouts, cabbage and cauliflower and the main hydroxycinnamic acids (sinapic, ferulic, p-coumaric and caffeic acids) were isolated by solid phase extraction with C18 cartridges. Using an optimised method, the four analytes were separated in less than 7 min in a 50 μm × 60 cm capillary with a 15 mM borate buffer (pH = 9.13) and a separation voltage of 30 kV at 30 °C. A linear relationship was observed for the method (r = 0.9997–0.9999) with detection limits ranging from 1.1 to 2.3 mg/kg of vegetables for the analytes. This method demonstrated good reproducibility with coefficients of variation of less than 5% for peak area and less than 1% for migration time (n = 7). The method was successfully applied to quantitatively determine the phenolic acid contents in a range of brassica vegetables and the results were in good agreement when compared to those from high performance liquid chromatography analysis.     

毛细管电泳安培检测法快速测定巧克力中的香兰素

运用毛细管电泳安培检测法研究了巧克力中香兰素的快速测定方法,研究了电极电位、缓冲液的浓度和pH、分离电压以及进样时间等因素对分离测定的影响。在30mmol/L的硼砂（pH9.24）运行缓冲液中,施加15kV的分离电压及+0.65V（vs.SCE）的电极电位条件下,铜电极对香兰素有很好的响应。香兰素在5.0×10-6～1.0×10-3g/mL范围内存在较好的线形关系,检测限为3.87×10-7g/mL（S/N=3）。对实际样品的测定,回收率为96.5%～102.8%,结果令人满意。      

Feasibility of using capillary zone electrophoresis with photometric detection for the trace level detection of bromate in drinking water

The feasibility of applying a capillary zone electrophoretic (CZE) method for the trace analysis of bromate, a suspect human carcinogen, in drinking water was studied. Using a bare fused-silica capillary (75 µm inner diameter) coupled with indirect ultraviolet detection (200 nm), 0.25 mM cetyltrimethylammonium bromide, 5% methanol and 5.0 mM phthalate at pH 5.0–5.2, an electrokinetic injection of 15 kV and 10 s, a separation voltage of 18 kV (negative polarity) and a capillary temperature of 15°C, bromate was detected in high purity water at ≤10 µg l^?1. The method was applied to three bottled water sources and to local municipal water. If needed, additional sample-handling steps, consisting of an off-line pre-concentration step and pH adjustment to 5.5, was used to improve detection limits (from a high of 400 µg l^?1 to ≤10 µg l^?1) and baseline noise. Signal-to-noise ratios also increased by adding sodium phosphate (1.1 µg ml^?1) to all sources prior to analysis. Although the CZE method was capable of detecting bromate at levels ≤10 µg l^?1 with an analysis time of 8–9 min, high variability (>10% relative standard deviation) precluded its application to some of sources without further method development. Nonetheless, this method could serve as the basis for the detection of bromate to specific water sources with minimal or no optimization     

毛细管电泳法同时检测南蛇藤中三种黄酮类活性成分

目的:建立同时测定南蛇藤中芦丁、山奈酚及槲皮素含量的毛细管电泳法,分析结果差异,探讨南蛇藤的药用质量控制方法。方法:采用30mmol·L-1硼酸钠缓冲液（pH=9.0）,20kV分离电压,254nm波长条件下采用毛细管电泳法测定芦丁、山萘酚、槲皮素含量。结果:黄酮类物质芦丁、山萘酚和槲皮素的对照品在12min内实现完全分离,在2.5⁴00μg·mL-1范围内呈良好的线性关系。结论:南蛇藤中黄酮类物质含量丰富,毛细管电泳技术可以同时测定南蛇藤中芦丁、山奈酚与槲皮素,具有较好的准确度和精密性,为临床和科研提供了一种简单快速的检测方法,为南蛇藤的药用质量控制提供了技术方法和理论数据。      

毛细管电泳法同时检测南蛇藤中三种黄酮类活性成分

目的:建立同时测定南蛇藤中芦丁、山奈酚及槲皮素含量的毛细管电泳法,分析结果差异,探讨南蛇藤的药用质量控制方法.方法:采用30mmol·L-1硼酸钠缓冲液(pH=9.0),20kV分离电压,254nm波长条件下采用毛细管电泳法测定芦丁、山萘酚、槲皮素含量.结果:黄酮类物质芦丁、山萘酚和槲皮素的对照品在12min内实现完全分离,在2.5～400μg· mL-1范围内呈良好的线性关系结论:南蛇藤中黄酮类物质含量丰富,毛细管电泳技术可以同时测定南蛇藤中芦丁、山奈酚与槲皮素,具有较好的准确度和精密性,为临床和科研提供了一种简单快速的检测方法,为南蛇藤的药用质量控制提供了技术方法和理论数据.