盐酸二甲双胍的毛细管电泳法快速测定

建立了毛细管电泳高频电导法快速测定片剂中盐酸二甲双胍的方法。考察了缓冲溶液、有机溶剂添加剂、毛细管长度以及分离电压和进样条件等因素对分离检测的影响。在最佳条件下5.0 min内即可实现盐酸二甲双胍分离检测,盐酸二甲双胍的线性范围为1.50μg/mL~130μg/mL,检出限为1.0μg/mL。该方法成功地测定了盐酸二甲双胍片剂中的盐酸二甲双胍。     

微芯片毛细管电泳法快速测定黄花鱼中的碱性嫩黄O

采用微芯片毛细管电泳非接触电导检测法,对黄花鱼中非法添加的工业染料碱性嫩黄O进行了分析。 探讨了缓冲液种类、浓度,分离电压和进样时间等因素对分离检测的影响。 实验选择5.0 mmol/L乳酸缓冲液(pH=3.29)、1.8 kV分离电压,在1.0 min内实现了碱性嫩黄O的快速分离测定。 在优化条件下,碱性嫩黄O浓度的线性范围为5.0～100.0 mg/L,黄花鱼中碱性嫩黄O的检出限为0.2 mg/kg,该法可成功测定黄花鱼中碱性嫩黄O的含量。     

微芯片毛细管电泳快速测定盐酸洛美沙星

采用微芯片毛细管电泳非接触电导检测法快速测定了盐酸洛美沙星胶囊中盐酸洛美沙星的含量。探讨了缓冲液类型、浓度,添加剂种类、浓度及分离电压、进样时间等因素对分离检测的影响。实验采用5.0mmol/L HAc(pH=2.5)+5%乙醇为缓冲溶液,分离电压3.0 kV,在1 min内实现了盐酸洛美沙星的快速分离测定。优化条件下盐酸洛美沙星的线性范围为20.0～250.0μg/mL,检出限为10.0μg/mL(S/N=3),RSD=2.0%,加标回收率为98.6%～103%。     

微芯片毛细管电泳快速测定加替沙星注射液中加替沙星的含量

研究了用微芯片毛细管电泳非接触电导检测系统快速测定加替沙星注射液中加替沙星的方法。对缓冲液的类型、浓度、分离电压以及进样时间等因素进行了优化。最佳条件为:缓冲液5.0 mmol/L HAc,分离电压2.0 kV,进样时间15.0 s。在该条件下,可在1.0 min内实现加替沙星的快速含量测定。线性范围为4.0～150μg/mL,检出限为1.0μg/mL,加标回收率为95.7%～101%,可成功测定注射液中加替沙星的含量。     

毛细管电泳法快速测定五倍子中的没食子酸

建立了毛细管电泳高频电导法测定没食子酸的方法.探讨了缓冲溶液、有机溶剂添加剂、分离电压等因素对分离检测的影响.在电泳介质为10.0mmol/L Tris-5.0 mmol/L H3BO3-15.0?H5OH,分离电压22.0 kV的优化条件下,5.5 min内即可实现没食子酸的分析,线性范围为3.00～100 μg/mL,检出限为1.0 μg/mL.成功地检测了五倍子中的没食子酸.     

毛细管电泳及芯片毛细管电泳的电容耦合非接触电导检测

综述了毛细管电泳(CE)及芯片毛细管电泳(MCE)的电容耦合非接触电导检测(Capacitively Coupled Contactless Conductivity detection,C4D)的研究状况;并分别对其装置、检测的影响因素及其应用进行了评述。引用文献81篇。     

毛细管电泳无接触电导检测研究进展

毛细管电泳(CE)电导检测(CD)是相对较灵敏和仪器结构简单的一项溶液分析技术,尤其是对于无生色团的无机离子分析更具有突出优势,因此,CE-CD技术近年来得到了较快发展[1],并已推出商品化的毛细管电泳电导检测器[2]。但CE和CD的偶联目前还存在如下几个问题:第一,加工适合于毛细管     

毛细管电泳法快速测定琥乙红霉素的含量

建立了毛细管电泳高频电导法测定琥乙红霉素的方法。探讨了缓冲溶液、有机溶剂添加剂以及分离电压和进样条件等因素对分离检测的影响。在电泳介质为2.0mmol/L柠檬酸-20.0?H5OH,分离电压20.0kV的优化条件下,在7min内即可实现琥乙红霉素的分离检测,线性范围为3.0μg/mL-150.0μg/mL,检出限为1.0μg/mL。方法简便、快速,可检测制剂中琥乙红霉素的含量。     

硫酸阿米卡星的毛细管电泳法快速测定

建立了毛细管电泳高频电导法快速测定注射液中硫酸阿米卡星的新方法.考察了缓冲溶液、有机溶剂添加剂以及分离电压和进样条件等因素对分离检测的影响.采用5.0 mmol/L乳酸-30%(体积分数)乙醇缓冲液体系为运行电泳介质,分离电压20.0 kV,在最佳实验条件下,5.5 min内即可实现硫酸阿米卡星的分离检测,硫酸阿米卡星的线性范围为5.00 ～150 mg/L,检出限为1.5 mg/L.     

芯片毛细管电泳非接触电导法快速测定葡萄糖氯化钠的含量

报道了一种芯片毛细管电泳-非接触电导法,用于快速测定葡萄糖氯化钠注射液中两种药物的含量。实验考察了运行缓冲液pH值和分离电压对组分分离的影响,以及检测器激励频率对组分信号响应和灵敏度的影响。确定以20 mmol/L硼酸缓冲液(pH 9.6)为分离介质,分离电压为1 200 V;最佳激励频率为70kHz。在上述条件下,两种成分(葡萄糖和Na+)可在60 s内实现有效分离。Na+和葡萄糖的线性响应范围分别为20～1 000μmol/L和50～5 000μmol/L(r≥0.992);按信噪比(S/N)为3∶1计算检出限分别为8.2μmol/L和26.7μmol/L。两个组分的回收率分别为95%～99%和97%～104%,相对标准偏差(RSDs)均小于4.0%。该文首次报道了葡萄糖和氯化钠两种常见药物成分的同时测定。方法简便、快速、准确度高、稳定性好,用于注射剂含量的测定,结果满意。     

芯片毛细管电泳电化学检测

评述了芯片毛细管电泳各种电化学检测尤其是安培检测中工作模式、工作电极、分离电流的消除、应用等方面的进展,并进行了展望。     

Contactless Conductivity Detection in Capillary Electrophoresis: A Review

The popularity of contactless conductivity detection in capillary electrophoresis has been growing steadily over the last few years. Improvements have been made in the design of the detector in order to facilitate its handling, to allow easy incorporation into available instruments or to achieve higher sensitivity. The understanding of its fundamental working principles has been advanced and the detection approach has also been transferred to lab‐on‐chip devices. The range of applications has been extended greatly from the initial work on small inorganic ions to include organic species and biomolecules. Concurrent determination of cations and anions by dual injection from opposite ends has been demonstrated as well as sample introduction by using flow‐injection systems for easy automation of the process.     

芯片毛细管电泳电化学发光法快速测定盐酸普鲁卡因的含量

建立了芯片毛细管电泳电化学发光法快速测定盐酸普鲁卡因含量的新方法。采用三联吡啶钌(Ru(bpy)2+3)为电化学发光试剂,三电极体系(直径300μm的铂圆盘电极为工作电极,集成在铂圆盘工作电极外的钛管为对电极,Ag/AgCl丝为参比电极)进行检测。分别考察了运行缓冲溶液pH值、检测缓冲溶液pH值、检测电位以及分离电压对分离和检测性能的影响。在优化条件下,即运行缓冲溶液为10mmol/L磷酸盐溶液(pH4.0),检测池缓冲溶液为含5mmol/LRu(bpy)2+3的50mmol/L磷酸盐缓冲溶液(pH7.0),检测电位为1.25V,分离电压为300V/cm时,盐酸普鲁卡因可在40s内实现较好的分离与检测,其线性范围为10~2000μg/mL(r2=0.9991),检出限(S/N=3)为3.0μg/mL,加标回收率为97%~99%,相对标准偏差为1.8%~2.2%。该方法简便、快速、准确,可用于盐酸普鲁卡因注射液的质量控制。     

毛细管电泳高频电导法快速分离检测混合氨基酸

氨基酸(Am ino acids,AA s)是组成生物大分子的基本单元,与人的健康状况有极其密切的关系.在医学和生命科学研究中,微量氨基酸的分离检测具有重要意义.     

微芯片毛细管电泳电化学/电化学发光同时检测药物分子

提出了基于毛细管电泳芯片的电化学和电化学发光同时检测技术.在此芯片系统中,三联吡啶钌Ru(bpy)₃²⁺[Tris(2,2'-bypiridyl) ruthenium(Ⅱ)]既作为电化学发光(ECL)检测所需的发光试剂与被分析物反应,生成激发态的Ru(bpy)₃^2+*,从而产生电化学发光信号;又具有催化作用参与电极表面的电化学反应,从而得到增强的电流响应.电化学信号与电化学发光信号同时产生并被分别纪录,从而实现了电化学和电化学发光的同时检测.这种芯片由两部分构成,分别是带有分离和进样通道的聚二甲基硅氧烷(PDMS)层和ITO(Indium tin oxide)工作电极底片.PDMS层与ITO电极底片采用可逆键合的方式组成芯片,该芯片大大简化了操作过程,提髙了发光信号的采集效率.在整个实验过程中,ITO电极表现出良好的稳定性,可长时间多次使用.选用山莨菪碱和氧氟沙星两种药物分子作为被分析物,对芯片系统性能进行了表征.     

Chiral Separation of Ofloxacin Enantiomers by Microchip Capillary Electrophoresis with Capacitively Coupled Contactless Conductivity Detection

We describe a chiral separation method for ofloxacin enantiomers, levofloxacin and dextrofloxacin by microchip capillary electrophoresis with capacitively coupled contactless conductivity detection. The running buffer included 1 mmol L^?1 MES and 1 mmol L^?1 Tris (pH 8.0) with a separation voltage of 1.5 kV and an injection time of 10s. Under these conditions, the enantiomers were completely separated within 1 min. The linear calibration curves were A = 5.76 c — 0.00587 for levofloxacin and A = 5.41 c — 0.00551 for dextrofloxacin, in which the linear concentration of the components all ranged from 0.05 to 0.15 mg mL^?1 (regression coefficients were both 0.9996). The limits of detection (S/N = 3) were, respectively, 18 and 21 μg mL^?1. The relative standard deviations of migration time were both 2.0% (n = 6). The relative standard deviations of peak area were 3.4% (n = 6) for levofloxacin and 4.0% (n = 6) for dextrofloxacin. The effects of some factors on resolutions, such as separation voltage and injection time, concentration of running buffers, were studied. The method was simple, rapid, high‐efficient. Furthermore, the method could be applied to the chiral separation of the product containing these enantiomers, such as Ofloxacin Eye Drops.     

左旋盐酸安妥沙星中对映体杂质的高效毛细管电泳法检测

建立了高效毛细管电泳检测盐酸安妥沙星中对映体杂质的方法。以含20 mmol/L HP-β-CD与70mmol/L磷酸二氢钾溶液(用磷酸调节pH3.0)为运行缓冲液,电压30 kV,柱温30℃,检测波长297 nm。可在10 min内将两对映体良好分离,检出限为2 mg.L-1(S/N=3),左旋安妥沙星在4.89~61.2 mg.L-1呈良好的线性关系,日内精密度(RSD)为2.1%(n=5),日间精密度(RSD)为3.2%(n=15)。     

Determination of heavy metal ions by microchip capillary electrophoresis coupled with contactless conductivity detection

An integrated detection circuitry based on a lock-in amplifier was designed for contactless conductivity determination of heavy metals. Combined with a simple-structure electrophoresis microchip, the detection system is successfully utilized for the separation and determination of various heavy metals. The influences of the running buffer and detection conditions on the response of the detector have been investigated. Six millimole 2-morpholinoethanesulfonic acid + histidine were selected as buffer for its stable baseline and high sensitivity. The best signals were recorded with a frequency of 38 kHz and 20 V(pp). The results showed that Mn(2+), Cd(2+), Co(2+), and Cu(2+) can be successfully separated and detected within 100 s by our system. The detection limits for five heavy metals (Mn(2+), Pb(2+), Cd(2+), Co(2+), and Cu(2+)) were determined to range from about 0.7 to 5.4 μM. This microchip system performs a crucial step toward the realization of a simple, inexpensive, and portable analytical device for metal analysis.