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.     

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。     

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.     

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.     

毛细管电泳法快速测定复方地芬诺酯片中的地芬诺酯和阿托品

建立了毛细管电泳高频电导法同时测定地芬诺酯和阿托品的方法。探讨了缓冲溶液、有机溶剂添加剂、分离电压和进样条件以及毛细管内径和长度等因素对分离检测的影响。在电泳介质为10.0mmol/L乳酸-15.0?H5OH、分离电压20.0kV的优化条件下,6min内即可实现地芬诺酯和阿托品的同时分离检测,线性范围分别为5.00~500和2.00~320mg/L;检出限分别为3.0和1.0mg/L。     

毛细管电泳高频电导法同时测定阿莫西林和克拉维酸钾含量

毛细管电泳高频电导法同时测定阿莫西林和克拉维酸钾含量;毛细管电泳; 高频电导检测; 非接触式电导检测; 阿莫西林; 克拉维酸     

毛细管电泳高频电导法测定制剂中卡托普利

建立了制剂中卡托普利毛细管电泳高频电导分析法,并用于卡托普利片、复方卡托普利片中卡托普利含量的测定。对电泳介质的种类、浓度以及操作电压和进样量等影响因素进行了优化。试验采用3.0 mmol.L-1环己胺+5.0 mmol.L-1H3BO3+0.50 mol.L-1乙醇作为电泳介质,20.0 kV为分离电压,可在8min内实现对卡托普利的分离检测。卡托普利的线性范围为5.0~550 mg.L-1,检出限为0.8 mg.L-1,回收率达95.5%~102.0%。     

牡丹皮中有效成分丹皮酚的毛细管电泳快速检测新方法

采用毛细管电泳高频电导法对丹皮酚进行了快速分离检测。对电泳介质的种类及浓度、操作电压和进样时间等影响因素进行了优化。最佳条件为：分离介质1．0mmol／LH3BO3-3．0mmol／L三乙胺-10％CH,OH（pH=8．0）,分离电压20．0kV,25．0cm位差虹吸进样8．0s。在该条件下。可在4min内实现对丹皮酚的分离检测。线性范围为2．0～105μg／mL,检出限为0．3μg／mL。成功测定了中药牡丹皮中的丹皮酚,回收率达94％～99％。方法简便、快速、灵敏,可用于药物分析。     

毛细管电泳测定甲芬那酸制剂及体液中的甲芬那酸

建立了制剂和体液中甲芬那酸毛细管电泳高频电导分析法,并用于甲芬那酸胶囊及血清、尿液中甲芬那酸含量的测定。对电泳介质的种类、浓度以及操作电压和进样量等影响因素进行了优化。实验采用3.0 mmol/L环己胺 3.0 mmol/LH3BO3 5.0mmol/Lβ-CD 0.17 mol/L乙醇作为电泳介质,20.0 kV为分离电压,可在7 min内实现对甲芬那酸的分离检测。在优化实验条件下,测定甲芬那酸的线性范围为0.8~550μg/mL,检出限为0.1μg/mL,回收率范围为98.3%~101.0%。     

毛细管电泳非接触式电导检测快速分离和测定氨基糖苷类抗生素

用带非接触式电导检测器的毛细管电泳法(CE)分离并测定了3种氨基糖苷类抗生素,即缺少较强紫外吸收发色团或荧光发射基团的庆大霉素(GE)、卡那霉素(KA)和链霉素(ST)。对影响CE分析的因素进行了研究,并确定以下几项优化的参数:①电泳介质:选用35mmol·L-12-(N-吗啉)乙磺酸溶液和15mmol·L-1组氨酸溶液组成的缓冲体系;②分离电压:17kV;③激发电压:60V;④激发频率:600kHz;⑤进样时间:5s。在所选最佳条件下,上述3种抗生素可在10min内达到完全分离。上述3种抗生素的质量浓度在一定范围内与其相应的峰面积呈线性关系,其检出限(3S/N)依次为0.2,0.4,0.2mg·L-1。     

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%。     

毛细管电泳高频电导法测定虫草中的有效成份

建立了毛细管电泳高频电导法同时测定腺苷和虫草素的方法。实验对电泳介质的种类、浓度以及操作电压和进样时间等因素进行了优化,在4mmol／L乳酸＋10％异丙醇＋80μg／mL羟甲基纤维素钠（pH=4．0）,分离电压20．OkV的条下测定了天然虫草和人工虫草菌丝制品中的腺苷和虫草素的含量,线性范围分别为2．0μg／mL～120μg／mL和3．0μg／mL～110μg／mL,检出限分别为0．5μg／mL和1．0μg／mL。     

Ultrafast capillary electrophoresis method for the simultaneous determination of ammonium and diphenhydramine in pharmaceutical samples

Ammonium and diphenhydramine are active ingredients commonly found in the same pharmaceutical preparations. We report, for the first time, a sub‐minute method for the simultaneous determination of ammonium and diphenhydramine. The method is based on capillary electrophoresis with capacitively coupled contactless conductivity detection. Both analytes can be quantified in a single run (∼80 injections/h) using 30 mmol/L 2‐(N‐morpholino)ethanesulfonic acid and 15 mmol/L lithium hydroxide (pH 6.0) as background electrolyte. The separation by capillary electrophoresis was achieved on a fused‐silica capillary (50 cm total length, 10 cm effective length, and 50 μm inside diameter). The limits of detection were 0.04 and 0.02 mmol/L for ammonium and diphenhydramine, respectively. The proposed method also provided adequate recovery values for spiked samples (100–106 and 97–104% for ammonium and diphenhydramine, respectively). The results obtained with the new capillary electrophoresis method were compared with those of the high‐performance liquid chromatography method for diphenhydramine and the Kjeldahl method for ammonium and no statistically significant differences were found (95% confidence level).     

Monosaccharide profiling of glycoproteins by capillary electrophoresis with contactless conductivity detection

Saccharides form one of the major constituents of biological macromolecules in living organisms. Many biological processes including protein folding, stability, immune response and receptor activation are regulated by glycosylation. In this work, we optimized a capillary electrophoresis method with capacitively coupled contactless conductivity detection for the separation of eight monosaccharides commonly found in glycoproteins, namely D-glucose, D-galactose, D-mannose, N-acetyl-D-glucosamine, N-acetyl-D-galactosamine, D-fucose, N-acetylneuraminic acid, and D-xylose. A highly alkaline solution of 50 mM sodium hydroxide, 22.5 mM disodium phosphate, and 0.2 mM CTAB (pH 12.4) was used as a background electrolyte in a 10 µm id capillary. To achieve baseline separation of all analytes, a counter-directional pressure of –270 kPa was applied during the separation. The limits of detection of our method were below 7 µg/ml (i.e., 1.5 pg or 1 mg/g protein) and the limits of quantification were below 22 µg/ml (i.e., 5 pg or 3 mg/g protein). As a proof of concept of our methodology, we performed an analysis of monosaccharides released from fetuin glycoprotein by acid hydrolysis. The results show that, when combined with an appropriate pre-concentration technique, the developed method can be used as a monosaccharide profiling tool in glycoproteomics and complement the routinely used LC-MS/MS analysis.     

Study on the effects of electrolytes and solvents in the determination of quaternary ammonium ions by nonaqueous capillary electrophoresis with contactless conductivity detection

A study on the separation of lipophilic quaternary ammonium cations in NACE coupled with contactless conductivity detection (NACE‐C⁴D) is presented. The suitability of different salts dissolved in various organic solvents as running electrolytes in NACE‐C⁴D was investigated. A solvent mixture of methanol/acetonitrile at a ratio of 90%:10% v/v showed the best results. Deoxycholic acid sodium salt as BGE was found to provide exceptional high stability with low baseline noise that leads to highest S/N ratios for the target analytes among all BGEs tested. Under the optimum conditions, capillaries with different internal diameters were examined and an id of 50 μm was found to give best detection sensitivity. The proposed method was validated and showed good linearity in the range from 2.5 to 200 μM, low limits of detection (0.1–0.7 μM) and acceptable reproducibility of peak area (intraday RSD 0.1–0.7%, n = 3; interday RSD 5.9–9.4%, n = 3).     

Determination of vitamin C and preservatives in beverages by conventional capillary electrophoresis and microchip electrophoresis with capacitively coupled contactless conductivity detection

The separation and detection of commonly used preservatives (benzoate, sorbate) and vitamin C by both conventional CE and microchip electrophoresis with capacitively coupled contactless conductivity detection is presented. The separation was optimized by adjusting the pH-value of the buffer and the use of hydroxypropyl-beta-CD (HP-beta-CD) and CTAB as additives. For conventional CE, optimal separation conditions were achieved in a histidine/tartrate buffer at pH 6.5, containing 0.025% HP-beta-CD and 0.1 mM CTAB. LOD ranged from 0.5 to 3 mg/L (S/N = 3) and the RSDs for migration time and peak area were less than 0.1 and 2%, respectively. A considerable reduction of analysis time can be accomplished by using microchip electrophoresis without significant loss in sensitivity under optimal separation conditions. A histidine/tartrate buffer at pH 6.5, incorporating 0.06% HP-beta-CD and 0.25 mM CTAB, gave detection limits ranging between 3 and 10 mg/L and satisfactory reproducibilities of < or =0.4% for the migration time and < or =3.5% for the peak area. The methods developed are useful for the quantitative determination of food additives in real samples such as soft drinks and vitamin C tablets.     

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。     

未衍生化卡托普利的毛细管电泳法测定

采用毛细管电泳高频电导法测定了未衍生化的卡托普利。考察了分离检测条件的影响。实验选择10．00mmoL／L Tris-5．0mmol／LH3BO3-20．0％CH3OH为电泳介质,在优化条件下,卡托普利的线性范围为1．00μg/mL-200μg／mL,检出限为0．3μg／mL。成功地检测了血清和尿液中的卡托普利。