黄芩及其制剂中黄芩素和黄芩甙的

用毛细管区带电泳 -电化学检测法测定了黄芩及其制剂中黄芩素和黄芩甙的含量。研究了电极电位、电解液酸度和浓度、电泳电压及进样时间等对电泳的影响 ,得到了较为优化的测定条件。以直径为300μm的碳圆盘电极为检测电极 ,电极电位为0.90V(vsSCE) ,在100mmol/L硼酸盐缓冲液(pH9.0)中 ,上述两组分在8min内完全分离。黄芩素和黄芩甙浓度与电泳峰电流分别在5.0×10 -7～1.0×10 -3mol/L和1.0×10 -6～1.0×10 -3mol/L范围内呈良好线性 ,检出限分别为2.24×10 -7mol/L和5.48×10 -7mol/L。7次测定分别含5.0×10 -4mol/L黄芩素和黄芩甙试样溶液 ,峰高的相对标准偏差分别为3.53%和4.03%。     

微波消解-毛细管电泳法测定茶叶中的生物碱

应用微波消解-毛细管电泳法测定3种茶叶中的咖啡因、腺嘌呤及儿茶素类化合物.优化了缓冲溶液体系、浓度、pH及分离电压等实验条件.在最佳实验条件下,以30 mmol/L硼砂-10 mmol/L β-环糊精为缓冲溶液,pH为9.0,分离电压为22 kV,检测波长为280 nm,电动进样20 kV×5s时,在7 min内同时分...     

Physicochemical characterization of phosphinic pseudopeptides by capillary zone electrophoresis in highly acidic background electrolytes

Phosphinic pseudopeptides (i.e., peptide isosteres with one peptide bond replaced by a phosphinic acid moiety) were analyzed and physicochemically characterized by capillary zone electrophoresis in the pH range of 1.1-3.2, employing phosphoric, phosphinic, oxalic and dichloroacetic acids as background electrolyte (BGE) constituents. The acid dissociation constant (pK(a)) of phosphinate group in phosphinic pseudopeptides and ionic mobilities of these analytes were determined from the pH dependence of their effective electrophoretic mobilities corrected to standard temperature and constant ionic strength of the BGEs. It was shown that these corrections are necessary whenever precise mobility data at very low pH are to be determined. Additionally, it was found that the ionic mobilities of the phosphinic pseudopeptides and pK(a) of their phosphinate group are affected by the BGE constituent used. The variability of migration behavior of the pseudopeptides can be attributed to their ion-pairing formation with the BGE components.     

Capillary electrophoresis with end-column amperometric detection of urinary 8-hydroxy-2'-deoxyguanosine

Urinary 8-hydroxy-2'-deoxyguanosine (8OHdG) is an excellent marker of oxidative DNA damage. Until now, urinary 8OHdG has been measured by high-performance liquid chromatography with electrochemical detection. A simple and sensitive method for the analysis of urinary 8OHdG by capillary electrophoresis with end-column amperometric detection has been developed in our laboratory. A single-step solid-phase extraction procedure was optimized and used for extracting 8OHdG from human urine. To improve the sensitivity of this method, a new focusing technique based on a dynamic pH junction was used. The limit of detection was 20 nM (signal-to-noise ratio S/N = 3), the linear range was 50 nM-10 microM, and the correlation coefficient was better than 0.999. The relative standard deviation (RSD) was found to be 0.57% for migration time, and 4.79% for peak current. To show the usefulness of the method, the urinary concentration of 8OHdG in nine healthy persons and ten cancer patients was determined. The urinary concentration of 8OHdG in cancer patients was significantly higher than that in healthy persons.     

Capillary gas chromatography of amines with ammonia as carrier gas

The use of ammonia as a carrier gas for the chromatography of aliphatic and aromatic amines has been investigated. As compared to nitrogen, ammonia gave drastically improved peak symmetry and lower capacity factors (k′) for primary and secondary amines on polar (Polyethylene glycol) and medium Polar (methylphenylcyanopropylsilicone) stationary Phases. The effect of ammonia was more Pronounced at low column temperatures. Considerably better detection limits of primary and secondary amines were obtained with ammonia as carrier gas than with nitrogen. No detrimental effects of using ammonia were observed on the gas chromatograph or on the columns over a period of about one year.     

Detection of paracetamol by capillary electrophoresis with chemiluminescence detection

Indirect detection of paracetamol was accomplished using a capillary electrophoresis-chemiluminescence (CE-CL) detection system, which was based on its inhibitory effect on a luminol-potassium hexacyanoferrate(III) (K₃[Fe(CN)₆]) CL reaction. Paracetamol migrated in the separation capillary, where it mixed with luminol included in the running buffer. The separation capillary outlet was inserted into the reaction capillary to reach the detection window. A four-way plexiglass joint held the separation capillary and the reaction capillary in place. K₃[Fe(CN)₆] solution was siphoned into a tee and flowed down to the detection window. CL was observed at the tip of the separation capillary outlet. The CL reaction of K₃[Fe(CN)₆] oxidized luminol was employed to provide the high and constant background. Since paracetamol inhibits the CL reaction, an inverted paracetamol peak can be detected, and the degree of CL suppression is proportional to the paracetamol concentration. Maximum CL signal was observed with an electrophoretic buffer of 30 mM sodium borate (pH 9.4) containing 0.5 mM luminol and an oxidizer solution of 0.8 mM K₃[Fe(CN)₆] in 100 mM NaOH solution. Under the optimal conditions, a linear range from 6.6 × 10⁻¹⁰ to 6.6 × 10⁻⁸ M (r = 0.9999), and a detection limit of 5.6 × 10⁻¹⁰ M (signal-to-noise ratio = 3) for paracetamol were achieved. The relative standard deviation (R.S.D.) of the peak area for 5.0 × 10⁻⁹ M of paracetamol (n = 11) was 2.9%. The applicability of the method for the analysis of pharmaceutical and biological samples was examined.     

N-(2-甲基-6-乙基苯基)丙氨酸对映体的毛细管电泳分离

采用高效毛细管区带电泳法,以β-环糊精及其衍生物作为手性选择剂,对外消旋N-(2-甲基-6-乙基苯基)丙氨酸(EMPA)的两个对映体进行了手性分离,比较了环糊精种类、环糊精浓度、电解质溶液pH值、温度和电场强度对分离的影响.实验结果表明,采用2,6-O-二甲基-β-环糊精为手性选择试剂,环糊精浓度为40mmol/L、电解质溶液pH=5.5及温度为20℃时分离效果最佳,对映体基本达基线分离,线性范围为20～200mg/L,最低检测限为10mg/L.     

Chiral separations by capillary electromigration techniques in nonaqueous media. II. Enantioselective nonaqueous capillary electrochromatography

A review on the advantages, peculiarities, and the potential of enantioselective capillary electrochromatography (CEC) in nonaqueous media is presented. Some fundamentals on CEC with particular focus on enantioselective CEC are discussed. The strategies, concepts, preferentially utilized chiral selectors and column technologies that have been utilized to succeed in highly efficient enantiomer separations by nonaqueous CEC are described thoroughly.     

Determination of barbituric acid and 2-thiobarbituric acid with end-column electrochemical detection by capillary electrophoresis

Capillary electrophoresis (CE) with end-column electrochemical detection (EC) of barbituric acid (BA) and 2-thiobarbituric acid (TA) has been described. Under optimum condition, BA and TA were separated satisfactorily, and a response of high sensitivity and stability was obtained at a detection potential of 1.25 V versus Ag/AgCl. Optimized end-column detection provides detection limit as low as 0.5 and 0.1 μM for BA and TA, respectively. The calibration graph was linear over three orders of magnitude. The relative standard deviations (n=10) of peak currents and migration times obtained for both BA and TA were 3.4, 3.7, and 1.7, 1.2%, respectively. The proposed method has been applied to analyze water sample with satisfactory results.     

Capillary complexation gas chromatography in analysis of cyclic and aromatic hydrocarbons

Summary Results of studies on stationary phases containing copper(II), nickel(II) and cobalt(II) chloride chemically bonded via cyano—or thiol groups are presented. The retention parameters—i.e. retention factor (k), retention index (I) and molecular retention index (ΔMe) and specific retention volume (Vg)-enabled the characteristics of specific interaction between aromatic and cyclic hydrocarbons and metal complexes chemically bonded to stationary phases to be determined. Presented at Balaton Symposium on High Performance Separation Methods, Siófok, Hungary, September 1–3, 1999