Determination of Chromate Ion in Water Using High Performance Capillary Electrophoresis

A new rapid method for the analysis of chromate ion in water by using high performance capillary electrophoresis is described. The detection limit is 1.0 mu g/ml by using 100 m mol/l Tris-HCl buffer containing 2 m mol/l 1,6-hexanediamine which was used as an electroosmosis modifier to improve the separation and detection sensitivity.

Analysis of Glutamic Acid in Cerebrospinal Fluid by Capillary Electrophoresis with High Frequency Conductivity Detection

A rapid method to determine glutamic acid (Glu) in cerebrospinal fluid (CSF) by capillaryelectrophoresis with high frequency conductivity detection (contactless conductivity detection) wasdescribed. The CSF sample was pretreated with silver cation resin to remove high concentration ofCl- ions in CSF. The separation was achieved in the buffer solution of 10 mmol/L Tris and 8mmol/L boric acid at the separation voltage of 20.0 kV. Glu showed linear response in the range of5.0×10-6 to 6.0×10-3 mol/L, the limit of detection was 1.0×10-6 mol/L. The method was used foranalysis Glu in CSF satisfactorily with a recovery of 97.8-98.8%.

Migration equation of solute in high performance capillary zone electrophoresis

In order to reveal the relationship between migration time and solute structure aswell as electrophoretic operation conditions in high performance capillary zoneelectrophoresis (HPCZE), researchers have presented many empirical and semi-empiricalmodels. These models have two main dissatisfactory points. Firstly, a constant is im-

Optimization strategies for separation of sulfadiazines using Box-Behnken design by liquid chromatography and capillary electrophoresis

Development of effective chromatographic or electrophoretic separation involves judicious deciding of selection of optimal experimental conditions that can provide an adequate resolution at a reasonable run time for the separation of interested components. Box-Behnken factorial design was effectively applied for the separation optimization of eight structurally related sulfonamides using capillary zone electrophorosis and reverse high performance liquid chromatography. Optimum values for volume ratio of THF to H2O in eluent, column temperature and flow rate of eluent are found as 12 to 88, 35℃ and 1.0 mL/min, respectively. Box-Behnken modified optimization model is extended to separation by capillary electrophoresis (CE). While using CE, a satisfactory separation is achieved with a minimum resolution larger than 1.0 for a separation time less than 10 min.

SEPARATION OF METAL IONS AS CHELATES OF 1N2,7O3,6S IN THE PRESENCE OR ABSSENCE OF TBA^+ BY CAPILLARY ELECTROPHORESIS

Separation and determination of metal ions based on the formation of chelate anions with 1-Nitroso-2, 7-dihydrexynaphthalene-3, 6-disulfonic acid (1N2, 7O3, 6S) was studied by rising HPCE of the nine metal ions examined, the ions that can be detected sensitively with 1-Nitroso-2, 7-dihydrexynaphthalene-3, 6-disulfonic acid were Fe2+, Co2+, Cu2+, Ni2+, Zn2+ and Pd2+. The cobalt chelate could exist in two oxidation states of cobalt. When TBA(+) were added in electrophoretic solutions, the drastic changes in elertrophoretic mobilities of chelate were observed, which was due to the ion association between chelates anions and TBA(+). The ion association constants of chelate anions with TBA(+) were determined by using the change in electrophoretic mobilities of chelates, metal ions tested were separated within 10 min using 30cm silica capillary (50 m i. d).

Quantitative Detection of Inositol Hexakisphosphate (InsP6) in Crop Plants Using Polyacrylamide Gel Electrophoresis (PAGE)

Inositol phosphates are essential for cell development and signaling in all living organisms. Inositol hexakisphosphate (InsP6) is the most abundant phosphoinositol in both plants and animals. While the concentration of inorganic phosphorous (Pi) is often limited in soil, some plants overcome this limitation by creating a phosphate reservoir that serves as a source of Pi during phosphate deficiency. Although this strategy benefits plant development and signaling under adverse environmental conditions, excessive accumulation of Pi in crop plants has raised serious concerns about its toxicity and ill effects on human health. Consumption of crop plants with high InsP6 content or food products made from these crops is found to reduce nutrient intake significantly by way of chelating essential metal cations in human and livestock fed by such plants. Therefore, it is necessary to determine InsP6 contents in crop plants. Several methods have been developed for the screening and detection of InsP6 in plants. These detection methods however, are complex, labor-intensive, and often provide inaccurate results. We have developed a fast, reliable, and cost-effective method for the detection and quantification of InsP6 in plants using polyacrylamide gel electrophoresis (PAGE) with potential applications in industry, quality control labs, and research projects.

Sensitive Method for Enantioseparation of Rivastigmine with Highly Sulfated Cyclodextrin as Chiral Selector by Capillary Electrophoresis

A sensitive method for enantioseparation of a basic drug rivastigmine and determination of its optical impurity by capillary electrophoresis with highly sulfated β-cyclodextrin （HS-β-CD） as the chiral selector is described. In general, enantioseparation of basic chiral compounds is carried out in acidic condition （pH 2.5） to prevent analytes from adsorption on the capillary wall. However, in the case of rivastigmine, the detection sensitivity was too limited to determine the optical impurity of S-rivastigmine lower than 1% when buffer pH was 2.5. It was found that the detection sensitivity was improved 1.6 times just by raising the buffer pH value from 2.5 to 5.8. The poor column efficiency due to the adsorption of the analytes on the capillary wall was resolved by using dynamical coating of the capillary wall with the linear polyacrylamide solution. The experimental parameters such as the concentration of HS-β-CD, buffer pH and buffer ionic strength were optimized, respectively. The method was validated in terms of repeatability, linearity, limit of detection （LOD） and limit of quantitation （LOQ）. Using the present method, the optical purity of nonracemic rivastigmine with the enantiomeric excess （ee） value of 99.14% was determined.

FLAT CAPILLARY ZONE ELECTROPHORESIS

Zone electrophoresis is suggested with flat capillary instead of circular ones to get over the disadvantages of both the narrow-bore and wlde-bore circular tubes (CT). This method was fully investigated in theory. A flat tube with a 2a×ka-mm (2a<ka) channel develops the maximum radial temperature gradient (π/k)-1 times less than an a -mm i. d. circular one. Compared with a 2a-ram i. d. circular tube, the flat one has at least a ((2k/π)-1)-fold increase in absorption response or decrease in detection limits, and the same fold increase in allowable sample throughput. The highest efficiency with a flat tube is thus expected. These were all tested in electrophoresis with 0.2×0.6-mm, 0.2-ram i. d. and 0.4-mm i. d. plastic tubes. Besides, the 0.2×0.6-mm flat tube required a less recovery time than the 0.2-mm i. d. tube and allowed a higher working voltage than the 0.4-mm i. d. tube, which implied that the flat tube offered the highest speed. The optimum k was observed at the values of 6—10 in the experiment and the recovery time was affected by the size of the tube and the viscosity of the solution.A preparation process of flat fluorocarbon polymer tubes is described in the paper, with a discussion on heat-deformatlon of the flattened tube.

Measurement and comparison of glycyrrhizic acid contents in root of licorice(Glycyrrhiza uralensis Fisch.)from different cultivating areas

The samples of licorice (Glycyrrhiza uralensis Fisch.) from 14 different cultivated areas were determined by the method of high Performance Capillary Electrophoresis (HPCE) for the contents of glycyrrihizic acid (GA) in root. The results showed that the licorice plants come from various cultivated areas of China has different contents of GA. The GA content of licorice from Zhaodong in Heilongjiang Province is the highest, followed by those from E抰uoke, Chifeng, and Hangjin Banner in Inner Mongolia. Some suggestions for establishing the production base of licorice were put forward based on the study.

基于PCR毛细电泳检测13种呼吸道病原体的性能验证

目的本研究旨在验证一种基于聚合酶链式反应(PCR)毛细电泳的13种呼吸道病原体多重检测试剂盒的主要性能。方法参照中国合格评定国家认可委员会(CNAS)的CNAS-GL039《分子诊断检验程序性能验证指南》,对13种呼吸道病原体多重检测试剂盒的准确性、特异性、最低检测限、抗干扰能力进行验证及评价。结果16个阳性参考品均检测出相应的病原体特征峰;特异性参考品未检测出病原体特征峰,未出现任何交叉反应;最低检测限参考品在24次重复检测中,结果均呈阳性;阳性标本在添加干扰物质的条件下,检测结果未受影响。结论基于毛细电泳的呼吸道病原体多重检测试剂盒可以准确、快速地检测出多种呼吸道病原体,其准确度、特异性、抗干扰能力、灵敏度均显示出良好的性能,符合产品要求,具有临床应用前景。

超高性能混凝土收缩研究进展

收缩是超高性能混凝土(UHPC)早期开裂的主要诱因,主要综述了UHPC收缩的发展规律、测试方法、调控手段及其收缩机理。结果表明:UHPC的收缩主要由自收缩和干燥收缩组成,而自收缩通常占总收缩的78.6%~90.0%,且主要集中在早期,后期收缩基本趋于稳定;热养护和组合养护可促进水泥水化以及掺合料的火山灰反应,改善孔结构,有利于消除后期UHPC收缩应变;毛细管张力理论可以很好地从相对湿度、孔隙结构、自应力、界面结构、水合程度来解释UHPC自收缩机理;当前UHPC收缩的测试方法主要侧重于实验室内,需要开发出一种实际工程应用中UHPC的收缩变形测量技术,实现可长期监测、数据实时传输、开裂的预报预警,对于大型工程UHPC结构的实时养护和工程防裂指导十分重要。

用于检测羧酸的基于高效毛细管电泳的微流控芯片

设计了一种可以进行高效毛细管电泳分析的微流控芯片,微流控芯片具有一个十字架结构的沟道,沟道横截面的尺寸为100μm×50μm。利用5-氨基甲基荧光素作为荧光探针,使用乙腈溶液与磷酸盐缓冲液作为流动相进行高效液相色谱分析,等量洗脱确认了丙酸到十八烷酸(C3~C18)的衍生物色谱图,并通过高效毛细管电泳分析将丙酸(C3)、己酸(C6)、癸酸(C10)进行分离,成功分离C3和C10,C3和C10的分离度为2.2,分离效果良好。此外,针对高效毛细管电泳分析出现的不稳定电渗现象而导致实验数据不稳定的情况,加入阳离子聚合物六甲溴铵和阴离子聚合物硫酸葡聚糖钠盐形成连续的多个离子聚合物涂层,使得微流控芯片对羧酸检测的稳定性大大提高。

Com parison of Amino Acids in Root Exudates of Flue-cured Tobacco Varieties with Different Resistances against Black Shank

In order to explore the differences of amino acids in root exudates and plant tissues, we selected four flue-cured tobacco varieties [ Yunyan 87 （ Ⅰ）, K326 （Ⅱ）, NC102（Ⅲ）, Hongda （Ⅳ）] as the test materials and studied the components and mass fractions of amino acids in rhizosphere soil, non rhizosphere soil, roots and leaves via high performance capillary zone electrophoresis. Ten amino acids were detected out from four varieties, including histidine, lysine, tryptophan, phenylalanine, valine, threonine, proline, serine, alanine and glycine. The mass fractions of amino acids in leaves and roots were higher than those in rhizosphere soil and non rhizosphere soil. In rhizosphere soil and non-rhizosphere soil, the mass fractions of lysine, phenylalanine, threonine, proline and glycine in susceptible varieties （ Ⅲ, Ⅳ） were higher than those in resistant varieties （ Ⅰ, Ⅱ）. In rhizosphere soil, the total amino acids successively were Ⅳ 〉 Ⅲ 〉 Ⅰ 〉 Ⅱ, and in non rhi- zosphere soil were Ⅲ 〉 Ⅳ 〉 Ⅰ 〉 Ⅱ. The total amino acids in roots of variety Ⅳ was the highest, up to 6 359. 195 μg/g. In leaves, the total amino acids in varieties I and If were higher than those in varieties IfI and IV. The results indicated that amino acids could secrete to rhizosphere via root secretion, and the compositions and mass fractions of amino acids varied with flue-cured tobacco varieties, thus the secretion amount of susceptible varieties was higher than that of resistant varieties.

毛细管电泳法测定桑叶中的黄酮类成分──芦丁和槲皮素

采用高效毛细管电泳法分离测定了新疆不同地区、不同采集期、不同品种的桑叶中的黄酮类成分芦丁、槲皮素的含量。以含有体积分数为 15 %甲醇的 10mmol/L的磷酸二氢钠 2 0mmol/L的硼砂溶液 (pH 8 6 2 )为电泳缓冲液 ,采用压力进样方式 ,在 2 5℃ ,2 0kV恒压下进行电泳分离 ,并在 2 45nm波长处检测。结果表明 ,桑叶中的两种目标组分在 12min内完全分离 ,且有良好的线性关系 ;芦丁和槲皮素的加样回收率分别为 95 6 4%和99 36 % ,其RSD分别为 2 2 5 %和 1 79% (n =6 )。方法简单、准确、快速。

高效毛细管电泳分离测定颠茄制剂中莨菪类生物碱

选择毛细管区带电泳分离模式，以麻黄素为内标建立了适合莨菪类生物碱阿托品、东莨菪碱、山莨菪碱、樟柳碱化化分离与颠茄酊剂及片剂定量分析的高效毛细管电泳方法。电泳分离条件：毛细管40c×50μm，运行缓冲液（pH8.0）50mmol／L磷酸盐溶液-四氢呋喃（9:1），电迁移进样5kV×5s，运行电压11kV（＋）→（－），柱上检测UV200um，0．02AUFS，毛细管柱温24℃。本法简便、快速、重现性好，可用于含莨菪类生物碱中药制剂的质量控制。

高效毛细管电泳法测定苦参碱和氧化苦参碱

建立了测定苦参碱和氧化苦参碱含量的高效毛细管电泳法。 ２０ ｍｍｏＬ／Ｌ的磷酸盐缓冲液（ｐＨ＝８．０）为电泳电解质，电压为３０ｋＶ（运行电流为１００～１１０ｕＡ），检测波长为２１４ｎｍ，内标氨茶碱。苦参碱 ０．１２６～１．２６ ｍｇ／ｍＬ、氧化苦参碱 ０．１０～１．０ ｍｇ／ｍＬ其浓度与峰面积之比呈良好的线性关系，ｒ均为０．９９９８，日内、日间变异系数均小于５．７％，常用２２种药物除地塞米松外其余的对其无干扰。用本法测定了２批苦参提取物，其中苦参碱为（４５．１９±０．０５８）％，（６２．８１±０．１２３）％；氧化苦参碱为（８．７１±０．０３）％，（６．８１±０．０８６）％。结果表明，该方法简单、灵敏，特异性和重现性良好，具有较强的实用价值。

中药菟丝子的高效毛细管电泳法鉴别

提取菟丝子种子植物蛋白用高效毛细管电泳法进行生药鉴定。实验表明，同属不同种菟丝子的碱溶性或酸溶性蛋白在成分和含量上均存在显著差异。根据其种子植物蛋白的电泳谱图，可有效地鉴别菟丝子的来源。运用此法对１３个生药样品进行了鉴定。

高效毛细管电泳法测定牛奶和奶粉中残留的三聚氰胺

建立了牛奶和奶粉中三聚氰胺的高效毛细管电泳-二极管阵列检测器(HPCE-DAD)检测方法。使用长度58.5cm、内径75μm的毛细管柱,分离电压25kV,进样量3.5kPa(35mbar)×8s,分离温度25℃,缓冲溶液20mmol/L柠檬酸-40mmol/L磷酸氢二钠(pH2.6),检测波长232nm。分析物在1～100mg/L范围内线性良好,r2>0.997;牛奶和奶粉的定量限分别为0.5mg/kg和1.0mg/kg。在添加水平为定量限浓度至50mg/kg时的回收率为72.2%～97.3%,相对标准偏差为2.1%～3.9%。

高效毛细管电泳法同时测定红花中腺苷、芦丁和槲皮素的含量

目的 用高效毛细管电泳法对红花中的有效成分腺苷、槲皮素和芦丁同时进行含量测定。方法 采用熔融石英毛细管柱 (66 5cm× 5 0 μmID ,有效长度 5 8cm)作为分离通道 ;以 5 0mmol·L- 1 硼砂其中含 18%甲醇的溶液 (pH9 7)为运行缓冲液 ;运行电压 :2 4kV ;毛细管柱温 :2 0℃ ;检测波长 :2 10nm。结果 以利福平为内标 ,腺苷、芦丁和槲皮素分别在 10～ 160mg·L- 1 ,10 0～ 2 0 0 0mg·L- 1 和 10 0～ 160 0mg·L- 1 线性关系良好 (r>0 998) ;平均回收率分别为98 5 %～ 10 0 5 % ,96 9%～ 99 5 %和 99 1%～ 99 5 % ;RSD分别为 6 5 % ,5 2 %和 5 6% (n =5 )。结论 此法操作简便快速 ,回收率及重现性好 ,可作为红花质量控制的方法。

芒果苷的高效毛细管电泳法分析

目的 :研究一种简便有效的芒果苷分离分析方法。方法 :利用高效毛细管电泳的自由溶液毛细管区带电泳 (CZE)技术分析从芒果树叶中提取的芒果苷。结果 :在波长 2 5 4nm可有效的检测Sigma和本实验室提取的两种来源的芒果苷 ,迁移时间相似。分别使用pH 6 .4,7.4和 8.4的 0 .0 5mol·L-1硼酸盐缓冲液和甲醇以 1∶0 .2 ,1∶0 .3,1∶0 .4,1∶0 .5混合作电泳缓冲液 ,发现以 pH7.4的硼酸盐缓冲液和甲醇以 1∶0 .3的比例混合作电泳缓冲液得到较好的分离效果 ,重复性好。结论 :CZE法分析芒果苷是一种简便、快速、成本低和效果好的方法 ,在临床药物分析中尤其适用。