pH区带逆流色谱法分离纯化马钱子中马钱子碱和士的宁

建立了pH区带逆流色谱分离制备马钱子中生物碱类成分马钱子碱和士的宁的方法。溶剂系统为V(甲基叔丁基醚):V(乙腈):V(水)=2:2:3,静置分层后,上相加入三乙胺,使其浓度为10mmol/L,作为固定相;下相加入HCl,使其浓度为10mmol/L,作为流动相。从308mg马钱子总生物碱中分离得到50mg马钱子碱和120mg士的宁,得率分别为72.8%和85.1%;纯度分别为96.8%和98.3%。并采用LC-ESI-MS和13CNMR对目标化合物的结构进行了鉴定。     

Determination of Dissociation Constants of Strychnos Alkaloids from Strychnos nux-vomica L. by Capillary Electrophoresis

An accurate capillary electrophoresis method was developed for the determination of dissociation constants of five Strychnos alkaloids from Strychnos nux-vomica L. The method relies on measuring the effective mobility of the solute as a function of the buffer pH. The mathematical relationship was strictly derived from the fundamental electrophoresis theory and the dissociation equilibrium of a weak base without any simplifications. Careful optimization of the running buffer permitted base-line resolution of the five structurally similar alkaloids.     

TLC Determination of Strychnine and Brucine of Strychnos nux vomica in Ayurveda and Homeopathy Drugs

Strychnos nux vomica is an important plant source for drugs of ayurvedic and homeopathic system of medicine. In this paper a thin layer chromatographic (TLC) method has been developed for the quantitative estimation of the two major alkaloids strychnine and brucine in the plant fruit and in ayurvedic and homeopathic drugs. Chloroform–ethyl acetate–diethyl amine (0.5:8.5:1) as mobile phase gave clear separation with no interference between the bioactive markers. The R _f values for strychnine and brucine were 0.55 and 0.42. The TLC method was found to be precise, rugged, robust and accurate with recovery of strychnine in the range 93.11–99.82% and brucine 96.95–99.48%. The limit of detection (LOD) and limit of quantification (LOQ) for strychnine were 1.9 and 8.25 ng and for brucine 2.2 and 9.2 ng respectively.     

Voltammetric Behavior of Strychnine, and its Determination in Strychno Nux-Vomica Seeds Extract

The voltammetric behavior of strychnine has been studied with a pyrolytic graphite (PG) electrode. The redox process taking place at the PG electrode is discussed. The cyclic voltammetric response has also been evaluated with respect to various experimental conditions, such as scan rate, pH of the supporting electrolyte, strychnine concentrations and accumulation time. A highly sensitive voltammetric method for the determination of strychnine is consequently developed. The linear calibration is in the range of 1×10⁻⁶ M – 1.1×10⁻⁴ M, with the limit of detection (LOD) being 1×10⁻⁸ M. The precision is excellent with a relative standard deviation (RSD) of 2.3%. The proposed cyclic voltammetric methodology has been applied to the determination of strychnine in the extract of Strychno nux-vomica seeds using the standard addition method. Consistent results have been obtained from both the electrochemical approach described here and the previously reported HPLC method.     

Determination of Active Ingredients of Origanum Vulgare L. and Its Medicinal Preparations by Capillary Electrophoresis with Electrochemical Detection

Abstract

A method based on capillary electrophoresis with electrochemical detection (CE‐ED) has been developed for the first time for the separation and determination of isovanillic acid, vanillic acid, quercetin, rosmarinic acid, caffeic acid, and protocatechuic acid in Origanum vulgare L. and its medicinal preparations. The effects of working electrode potential, pH level, concentration of running buffer, separation voltage, and injection time on CE‐ED were investigated. Under the optimum conditions, the analytes could be separated in a 50 mmol L^?1 borate buffer (pH 8.7) within 21 min. A 300‐µm diameter carbon disk electrode has a good response at +0.95 V (vs. SCE) for all analytes. The response was linear over three orders of magnitude with detection limits (S/N=3) ranging from 4×10^?8 g mL^?1 to 2×10^?7 g mL^?1 for the analytes. The method has been successfully applied to the analysis of real sample, with satisfactory results.     

毛细管电泳法测定双氢青蒿素的含量

使用自行设计的毛细管电泳柱端安培检测系统,在乙醇为有机添加剂的条件测定了双氢青蒿素。研究了工作电极、缓冲溶液浓度及其pH、有机溶剂的选择及其含量、检测电位和分离高压对测定的影响。结果表明：选用Ag工作电极,检测电位为-O．6V,在20mmol／L硼砂,pH为9的运行介质的优化条件下,双氢青蒿素在4min左右出峰,在1～200mg/L范围内,峰高与浓度呈良好的线性关系,检出限为O．05mg/L。     

Determination of Taurine in Lycium Barbarum L. and Other Foods by Capillary Electrophoresis with Electrochemical Detection

A method based on capillary electrophoresis (CE) with electrochemical detection (ED) was developed for the determination of taurine in Lycium Barbarum L., LIPOVIYAN beverage and milk powder. The effects of some important factors such as the acidity of the running buffer, separation voltage, injection time, and applied potential to working electrode were investigated. Operated in a wall‐jet configuration, a 300 μm diameter carbon‐disk electrode was used as the working electrode, which exhibits good responses at +1.05 V (vs. SCE) for taurine. Excellent linearity was obtained in the concentration range from 5.0×10^?4 mol/L to 5.0×10^?6 mol/L. The detection limit (S/N=3) was 1.0×10^?7 mol/L. This proposed method has been successfully applied to analyze the actual samples with satisfactory assay results.     

Determination and Differentiation of Two Seemingly Identical Medicinal Herbs by Capillary Electrophoresis with Electrochemical Detection

A high-performance capillary electrophoresis with electrochemical detection (CE-ED) method has been employed for the determination of six bioactive ingredients in traditional Chinese herbs, Herba cepbalanoplosis segeti and Herba cirsii japonici. 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 CE-ED were investigated. Under the optimum conditions, the six analytes could be well separated within 21 min in a 75 cm length capillary at the separation voltage of 15 kV in a 50 mmol L^–1 borax running buffer (pH 8.4). A 300 m diameter carbon disk electrode was used as the working electrode positioned carefully opposite the outlet of the capillary in a wall-jet configuration at potential of +950 mV (vs. SCE). Good linear relationship was established between peak current and concentration of analytes over two orders of magnitude with detection limits (S/N=3) ranged from 1.5×10^–7 to 6.0×10^–7 g mL^–1 for all six analytes. This proposed method has been successfully applied for the analysis of traditional Chinese herbs after a relatively simple extraction procedure, further on, for the differentiation of these above two seemingly identical herbs based on their electropherograms or characteristic electrochemical profiles.     

非水介质毛细管电泳高频电导法测定姜黄中姜黄素

建立了药材姜黄中姜黄素含量的非水介质毛细管电泳高频电导测定方法.对非水介质体系和支持电解质的种类,浓度以及操作电压和进样时间等影响因素进行了优化.以无水甲醇作为分离介质,NH4OAc-HOAc为电解质,25.0 kV为分离电压,可在12 min内实现对姜黄素的分离检测.在最佳试验条件下,姜黄素的线性范围为3.0～140.0 mg·L-1,检出限为0.5 mg·L-1,回收率为95.3%～100.9%.     

毛细管电泳电化学检测单糖的研究

采用毛细管区带电泳直立式安培电化学检测方法分离和测定单糖。考察了电解质溶液的ＰＨ和浓度对单糖分离的影响，适量加入氯化钠可改善分离条件。应用该法进行了乳糖的组成和人血中葡萄糖的测定。     

高效毛细管电泳电导法测定青蒿素的含量

建立了青蒿中青蒿素含量测定的高效毛细管电泳-电导法,Tris—H3BO3（H3BO3浓度为1．5mmol／L）为电泳介质,乙醇为有机添加剂,在15kV高压,pH9．0的碱性条件下柱端电导法检测了青蒿中的青蒿素含量,着重探讨了缓冲溶液种类、浓度、酸碱度及其操作电压、进样时间对检测的影响。该法的线性范围为20-280mg／L,检出限为3．2mg／L;结果表明该法简便、快速、准确,适用于青蒿素含量的测定。     

Separation and Determination of Eremophilenolides from Ligulariopsis shichuana by Capillary Zone Electrophoresis

A new method of capillary zone electrophoresis (CZE) was established by simultaneous assay of four eremophilenolides, 3β-acetoxy-9β-angeloyloxy-1β,10β-epoxy-8α-hydroxyeremophil-7(11)-en-8β (12)-olide (1), 3β-senecioyloxy -1β,10β-epoxy-8α-hydroxyeremophil-7(11)-en-8β (12)-olide (2), 6α-hydroxy-1β,10β-epoxy-8α-hydroxyeremophil-7(11)-en-8β (12)-olide (3) and 3β-acetoxy- 6β-angeloyloxy-1β,10β-epoxy-8α-hydroxyeremophil-7(11)-en-8β (12)-olide (4) in the Chinese herbal extract from Ligulariopsis shichuana. The optimum buffer system was 20 mM borate buffer (pH 10.00). Voltage was 25 kV and detection at 214 nm. Regression equations revealed linear relationships (correlation coefficients 0.9986, 0.9990, 0.9992 and 0.9995) between the peak area of each compound and its concentration. The relative standard deviations of migration times and peak areas were <1.35 and 3.94% within 1 day, respectively. The effects of several CE parameters on the resolution were studied systematically. The contents of four eremophilenolides in Ligulariopsis shichuana were successfully determined with satisfactory repeatability and recovery.     

毛细管电泳-电化学检测法测定中药杠版归中的活性成分

采用毛细管电泳-电化学检测法（CE-ED）同时分离测定了中药杠板归中的阿魏酸、香草酸、槲皮素、咖啡酸、原儿茶酸等主要生物活性成分的含量。考察了工作电极电位、运行缓冲液的pH值和浓度、分离电压和进样时间等实验参数对实验结果的影响。在优化的实验条件下,以直径300 μm的碳圆盘电极为工作电极,检测电位为＋0.95V(vs. SCE),在10mmol/L磷酸盐（pH 9.2）的运行缓冲溶液中,五个分析物能够在17min内实现很好的基线分离,被测物浓度与峰电流在3个数量级呈良好的线性,检测限（S/N＝3）范围从7.1×10-8 到 9.3×10-8g mL-1。该方法已应用于实际样品的分析,样品处理简单,获得了令人满意的结果。     

Chiral Separation of Ibuprofen and Terbutaline by Nonaqueous Capillary Electrophoresis with Conductance Detection

IntroductionThe separation of chiral substances is a chal-lenge task to analytical chemistry and pharmaceuti-cal chemistry.HPLC[1] and GC[2 ] are the commonchiral separation techniques.Unfortunately,theyare time- consuming and strenuous.In addition,thechiral separation columns are expensive and thebaseline separation is hard to be obtained.Recently,the researches of chiral separationwith capillary electrophoresis have been active[3 ,4 ] .However,the instrument with an optical detectorcosts …     

茶叶中无机阴离子的毛细管电泳分离间接检测方法的研究

建立了毛细管电泳分离测定茶叶中Cl-、NO2-、NO3-、SO42-、F-及HPO24-的方法。通过研究分离电压、背景电解质和电渗流改性剂的浓度、pH的影响优化了分析条件。在优化条件下,6种无机阴离子在10min内得到完全分离,各组分迁移时间和峰高的相对标准偏差(RSD)分别为1.9%~4.7%和1.2%~3.8%,检出限为0.11~0.82 mg/L。通过分析实际样品并做加标回收实验验证了该方法的可行性,Cl-、NO3-、SO42-及HPO24-的回收率为93%~98%。     

非水体系毛细管电泳-紫外检测法测定对乙酰氨基苯酚的研究

本文报道了用非水相体系高效毛细管电泳-紫外检测法测定对乙酰氨基苯酚的新方法;考察了运行电压、非水相介质和电解质等因素的影响。在25℃下,以50mmol／L NaOH的乙醇溶液为电泳缓冲介质,30mmol／L乙酸钠的乙醇溶液为样品溶剂;选择重力进样30S,运行电压-25kV,及检测波长250nm。测定对乙酰氨基苯酚的线性范围为5．2～52μg／mL;检出限为2．88μg／mL;RSD为2．34％。本法应用于维C银翘片中对乙酰氨基苯酚的测定,结果满意。     

毛细管电泳定量检测环境水样中无机阴离子

详细讨论了胶束浓度、间接吸收背景物质的浓度及有机添加剂组成等对部分卤素及其含氧酸根的毛细管电泳分离影响;在优化的条件下,3.5min内高效、快速地完成了Cl-、Br-、ClO3-、BrO3-四种无机阴离子的分离分析,分离的理论塔板数在1.6×106～2.8×105/m之间,检出限在11.2～23.3mg/L之间,迁移时间的相对标准偏差小于1%,峰面积的相对标准偏差在5.2%～2.2%之间;并将方法用于环境水样的分析。     

Determination of Podophyllotoxin and 4′-Demethylepipodophyllotoxin by Capillary Electrophoresis

A new simple, rapid and sensitive capillary zone electrophoresis (CZE) method has been developed for the simultaneous separation and determination of the anticancer active compounds podophyllotoxin (PPT) and 4′-demethylepipodophyllotoxin (DMEP) in ethanol extracts of the roots of Sinopophyllum emodi (Wall) Ying, and the roots, stems, leaves and fibrils of Dysosma versipellis (Hance) M. cheng. PPT and DMEP could be completely separated and sensitively determined at 214 nm within 12.5 min using 25 mM borate with pH 10.80 as running buffer (applied voltage 20 kV, temperature 20 °C, injection time 5 s). The linear range for the determination of PPT and DMEP were 1.5–171.0 μg mL⁻¹ and 5.0–136.0 μg mL⁻¹ with RSD of the relative migration time for PPT and DMEP of 1.50 and 3.26, and of the relative peak area of 0.82 and 1.13, respectively. The results showed that the method had requisite selectivity, sensitivity, reproducibility and wide linear range for the application to the rapid separation and accurate determination of PPT and DMEP in podophyllum plants. Furthermore, this is the first report about the analysis of podophyllotoxin analogues by CE.     

爆炸残留物的毛细管电泳检测

1引言爆炸是恐怖袭击的常用手段。对痕量爆炸残留物进行高效检测,从而准确判断炸药的成分和种类,能够为侦破案件提供重要的线索和证据[1,2]。近年来,毛细管电泳技术初步显示了其在爆炸物检验方面的巨大潜力[3～6]。本实验基于毛细管电泳间接紫外吸收检测[7,8]和胶束电动色谱[9],建立了痕量爆炸残余物的系统分析检验方法,通过对爆炸瞬间产生的痕量     

烟草中糖类物质的高效毛细管电泳-安培检测研究

将高效毛细管电泳－安培检测技术（ＨＰＣＥ－ＡＤ）用于不同烟草样品中糖类物质的测定。在 １×１０－６ｍｏｌ／Ｌ～１×１０－３ ｍｏｌ／Ｌ范围内,存在良好的线性关系,葡萄糖、果糖、蔗糖和麦牙糖的检测限均小于 ５．０ ×１０－７ｍｏｌ／Ｌ,结果令人满意。