毛细管胶束电动色谱法分离和定量5种喹诺酮类药物

建立了５种喹诺在药物的毛细管胶束电动色谱分离和尿样品的定量测定方法。测定条件为：运行缓冲液：５０ｍｍｏｏｌ／Ｌ磷酸二氢钠－１００ｍｍｏｌ／Ｌ溴化十六烷基三甲胺（１：１,ｐＨ４．５）,操作电压１２ＫＶ,检测波长２８０ｎｍ,２０ｍｉｎ内５种喹诺酮药物全部得到分离,并与毛细管区带电泳作了比较。尿液对样品的测定无干扰。线性范围为５．０～３５．０ｍｇ／Ｌ,最低检测浓度为２ｍｇ／Ｌ,ＲＳＤ小于１０％。     

毛细管电泳法分离硝基喜树碱的同分异构体

目的 :建立分离硝基喜树碱同分异构体的毛细管电泳分析法。方法 :用未涂渍熔融石英毛细管 ( 4 8.5 cm× 5 0 μm,有效长度 40 cm) ,以 40 mmol/L 硼砂 -4 0 mmol/L十二烷基硫酸钠、溶剂以水∶甲醇 =9∶ 1(磷酸调节 p H=8.0 )为缓冲液 ,运行电压 2 0 k V,温度 2 5℃ ,检测波长 2 40 nm。结果 :硝基喜树碱的一对同分异构体能够达到基线分离。 p H值和电压对其分离度影响较小 ;温度和 SDS的浓度对其分离度影响较大。 结论 :此方法可用于硝基喜树碱同分异构体的分离分析。     

胶束电动毛细管色谱法分析替考拉宁

目的建立毛细管电泳分离替考拉宁各主要组分的新方法。方法通过表面活性剂的浓度、缓冲液的浓度及pH、温度及电压的优化,选择最佳的分离条件。结果最佳分离条件硼酸盐∶磷酸二氢钠缓冲液(40mmol/L硼砂,10mmol/L磷酸二氢钠,用硼酸调节pH9.35,内含0.35%十二烷基硫酸钠);检测波长214nm,电压30kV,30℃,基线分离了替考拉宁的主要组分,并对所建立的新方法进行了方法学验证。结论建立的毛细管电泳法实用性强,费用低,为该品种的质量控制提供了一种可选择的新方法。     

反相离子对高效液相色谱法和高效毛细管电泳法测定春雷霉素

用建立的反相离子对高效液相色谱法和高效毛细管电泳法对春雷霉素发酵液、提炼液和原粉进行了含量测定,并对两种分析方法进行了比较。实验表明,两种方法之间不存在差异,测定结果一致。通过方法的验证,证实了两种方法都适合于春雷霉素的分析测定。     

毛细管电泳法分离测定血浆样品中盐酸多奈哌齐对映体

目的分离、测定血浆样品中盐酸多奈哌齐对映体的含量。方法建立高效毛细管电泳法血浆中加入内标L-酒石酸布托菲诺后，碱化并以异丙醇-正己烷(3∶97)提取血浆样品，采用未涂层熔融石英毛细管柱(70 cm×50 μm ID)，以25 mmol·L^-1磷酸-三乙胺(pH 2.5)为运行缓冲液，2.5%磺化β-环糊精为手性添加剂，进样电压为-20 kV，进样时间为15 s，运行电压为-20 kV。对盐酸多奈哌齐对映体进行电泳分离，并进行家兔血浆样品中盐酸多奈哌齐对映体定量分析的方法验证。结果在上述电泳条件下，盐酸多奈哌齐对映体可达基线分离。测得血浆样品中R(-)-多奈哌齐的回归方程为：A_s/A_i=0.024 2+0.289 2C，r=0.999 2，S(+)-多奈哌齐的回归方程为：A_s/A_i=0.010 8+0.273 7C，r=0.999 7，线性范围为0.1～5 mg·L^-1，检测限为0.05 mg·L^-1。结论本法与手性柱HPLC法相比，有高效、快速和经济等优点。     

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。     

毛细管区带电泳法测定单唾液酸神经节苷脂GM_1的含量

目的建立毛细管区带电泳法分离测定单唾液酸神经节苷脂GM1 的方法。方法采用熔融的硅胶毛细管柱 (90cm× 75 μm ,有效长度为 83cm) ,以含 1 5mmol/L浕 环糊精的 2 5mmol/L硼砂缓冲液为电极缓冲液 (pH 9.4 ) ,检测波长 :2 0 0nm。结果GM1 线性范围为 0 .0 4 2～ 4 .2 3mg/ml(r =0 .9981 ) ,回收率 (n =3)分别为 98.85 % (RSD =1 .7% )、99.0 6 % (RSD =1 .1 % )、99.0 1 % (RSD =1 .2 % )。结论此法简便、快速、准确 ,适用于该药品的生产及临床应用中的质量控制     

区带毛细管电泳法分离测定莨菪浸膏片中莨菪烷类生物碱

目的:建立区带毛细管电泳法分离测定莨菪浸膏片中4种良菪烷类生物碱——阿托品、山茛若碱、樟柳碱和东茛若碱的含量。方法:以50μm×50.0 cm(有效长度37.5 cm)的毛细管为分离通道,工作电压25 kV,温度25℃,压力进样:21 Pa×5 s,100 mmol·L Tris-磷酸(pH 8.6)为背景电解质,检测波长202 nm。结果:硫酸阿托品、氢溴酸山莨菪碱、樟柳碱和氢溴酸东莨若碱浓度分别在2.05～41.04μg·mL~(-1)(r=0.9982),2.04～40.72μg·mL~(-1)(r=0.9958),2.05～41.0μg·mL~(-1)(r=0.9965),2.13～41.60μg·mL~(-1)(r=0.9974)的范围内呈良好的线性关系;平均回收率分别为99.2%,98.5%,95.1%,98.2%。结论:此方法快速、简使、准确,可作为茛菪浸膏片的质量控制方法。     

A method for the determination of minoxidil in hair-regrowth formulations by micellar electrokinetic capillary chromatography

A method based on micellar electrokinetic capillary chromatography (MEKC) was developed for determination of minoxidil in Rogaine and competing products. The original intent of the work was to offer an orthogonal means to HPLC for testing illicit imitations of Rogaine. However, because the patent has since expired, we offer the procedure as a confirmatory measure to HPLC for assay of generic minoxidil products. The MEKC procedure complements an earlier method based on free solution capillary electrophoresis (FSCE), designed to the same end. Validation was carried out on both a Dionex CES-1, which utilizes gravity injection, and a PE-ABI 270HT, which employs vacuum injection. The procedure was validated for both active pharmaceutical ingredient and for minoxidil solutions. The run buffer is pH 7.0, 20 mM sodium phosphate, 20 mM sodium dodecyl sulfate, with 10% isopropanol; the internal standard is dl-tryptophan. The method bears the attributes of simplicity, ease of use, and short analysis time (12 min). It is selective with respect to known process and degradation impurities. High efficiency was achieved on the CES-1, with a plate count exceeding 200,000 for minoxidil at an elution time of 9 min. Although slight differences in performance were noted across the two instruments, results on both were in conformance with modern day validation expectations. Comparison of MEKC with HPLC resulted in slightly higher values for the former, but all results met registration specifications and internal targets.     

胶束电动毛细管电泳法分离6种生物碱基

目的:采用胶束电动毛细管电泳法(MECC)分离腺嘌呤(A)、鸟嘌呤(G)、胞嘧啶(C)、胸腺嘧啶(T)、茶碱和咖啡因6种生物碱基。方法:20℃、18 kV 应用电压下,检测波长270 nm,在 35 mmol·L~(-1)十二烷基硫酸钠(SDS)-10 mmol·L~(-1)硼砂(pH 9.0)运行缓冲液中电泳分离。结果:6种碱基8 min 内达到基线分离;在10～500 mg·L~(-1)浓度范围内呈良好线性关系;相关系数为0.9995～0.9999;检出限为12.5～100μg·L~(-1),加样回收率在96.1%～105.2%。并用于3种药物和茶叶中生物碱基含量的测定。结论:方法简便、快速,灵敏度高,可用于分析和测定含生物碱基的药物和饮料。     

毛细管电泳法分离分析去甲肾上腺素等单胺类神经递质及肾上腺素

利用毛细管电泳法分离去甲肾上腺素 ,5 -羟色胺以及多巴胺三种单胺类神经递质以及肾上腺素。采用自由区带电泳法 ,4 0mmol/L硼砂缓冲液 2 0PSI气压进样 5s,定电压 2 0KV分离 12min。结果显示四种物质完全分离     

Separation and determination of the effective components in the alabastrum of Edgeworthia chrysantha Lindl. by micellar electrokinetic capillary chromatography

A rapid and efficient micellar electrokinetic capillary chromatography (MEKC) method was developed to analyze edgeworoside C (1), kaempferol-3-O-beta-D-glucoside (2) and rutin (3) in the alabastrum of Edgeworthia chrysantha Lindl. for the first time. The factors that affect the separation were studied, such as the concentrations of the buffer, SDS, and organic modifier, the apparent pH, the applied voltage and temperature. The analytes were well separated within 15 min with an electrolyte containing 25 mM Na(2)B(4)O(7), 30 mM NaH(2)PO(4), 60mM SDS and 15% acetonitrile (pH(*) 9.1) at 25 kV and 15 degrees C. The correlation coefficients between the peak areas of analytes and the corresponding concentrations were 0.9976-0.9981 under the optimum conditions. The relative standard deviations (R.S.D.) of the migration time and peak area were in the range 0.6-1.7 and 1.9-5.3%, respectively. The contents of analytes in E. chrysantha Lindl. collected from the different places were successfully determined with the recoveries ranging from 95.9 to 104.3%. And, the results demonstrated that there was significant difference between the two real samples.     

盐酸去甲万古霉素的高效液相色谱和胶束电动毛细管色谱分析

建立了高效液相色谱(HPLC)法和胶束电动毛细管色谱(MECC)法测定盐酸去甲万古霉素中去甲万古霉素的含量。色谱条件HPLCKromasilC18柱;流动相A0.3mol/L甲酸铵溶液(pH7.5)-水(15∶85),B0.3mol/L甲酸铵溶液(pH7.5)-二氧六环(15∶85);梯度洗脱;柱温35℃;检测波长280nm;MECC熔融石英毛细管柱;背景电解质含0.06mol/L十六烷基三甲基溴化铵的0.12mol/L三羟甲基氨基甲烷-磷酸盐缓冲液(pH3.0);外加电压-15kV;柱温25℃;检测波长220nm。采用本文的HPLC和MECC方法,去甲万古霉素与有关物质尤其是与主要杂质之间的分离较好。HPLC方法和中国药典方法对暂行国家标准品和2批供试品中去甲万古霉素含量的测定结果一致。由于此前在标定暂行标准品时所用色谱系统未能分离出主要未知杂质,因而标准品的去甲万古霉素含量的标示值明显偏高,且测定结果揭示该批标准品中去甲万古霉素的含量显著低于中国药典的规定,故建议有关部门制备新的盐酸去甲万古霉素国家标准品。     

Separation of diastereomeric anthrone-C-glucosyls of aloes by micellar electrokinetic capillary chromatography

The anthrone-C-glucosyls aloin A and B, 5-hydroxyaloin A, 10-hydroxyaloin A and B were separated by micellar electrokinetic capillary chromatography (MECC) with sodium dodecyl sulfate in borate buffer pH 9 within less than 7 min. The method has been successfully transferred to the analysis of the two European Pharmacopoeia drugs Cape aloes and Cura?ao aloes. A comparison of the peak areas received by HPLC and MECC indicated the transferability of the measured contents.     

非水毛细管电泳法分离分析非甾体抗炎药物

目的建立一种非水毛细管电泳法(NACE)分离非甾体抗炎药物,并对奥沙普秦肠溶片进行定量分析。方法以含醋酸铵15mmol/L的甲醇-乙腈(3∶7)混合液为电泳缓冲液,运行电压20kV,柱温20℃,进样压力2.5kPa,进样时间10 s,UV检测波长200nm;内标法(内标:布洛芬)定量奥沙普秦肠溶片。结果NACE能有效分离布洛芬、萘普生、奥沙普秦、舒林酸和双氯芬酸钠五种非甾体抗炎药物。奥沙普秦与布洛芬的峰面积比对奥沙普秦浓度C(μg/mL)的线性回归方程为Y=0.0434C-7.1×10-3(R=0.999 9,n=9),线性范围0.8~80μg/mL,加样回收率99.05%~101.48%,日内、日间精密度分别为0.54%~0.83%,0.55%~0.92%。结论NACE用于奥沙普秦等非甾体抗炎药物的分离分析,选择性高,重现性好,准确,快速,可作为该类药物及其制剂的质量控制手段。     

胶束电动毛细管色谱法测定金果榄中古伦宾和蝙蝠葛任碱的含量

目的建立测定金果榄药材中古伦宾和蝙蝠葛任碱含量的胶束电动毛细管色谱法。方法采用未涂层熔融石英毛细管柱(35.2 cm×50μm I.D.,有效长度为26.9 cm),运行缓冲液为20 mmol.L-1硼酸溶液(含200 mmol.L-1十二烷基硫酸钠,pH值8.0)-异丙醇-甲醇(体积比70∶20∶10),分离电压为18 kV,检测波长为210 nm,压力自动进样。结果古伦宾和蝙蝠葛任碱的线性范围分别为0.210～1.68 g.L-1和0.026～0.21 g.L-1,线性关系良好。平均加样回收率分别为100.5%和96.1%,RSD分别为3.4%和3.6%(n=6)。应用该法测定10批金果榄药材中古伦宾和蝙蝠葛任碱的含量。结论该方法准确、可靠、环保,适用于金果榄中古伦宾和蝙蝠葛任碱的同时含量测定。     

胶束毛细管电泳法测定牛磺酸滴眼液中的羟苯乙酯

目的建立一种简便快速的胶束毛细管电泳法测定滴眼液中的抑菌剂羟苯乙酯的方法。方法采用未涂层石英毛细管柱(50μm×50 cm,有效分离长度41 cm)为分离通道,采用紫外检测器,检测波长254 nm,以20 mmol.L-1硼酸盐(pH7)-10mmol.L-1 SDS为运行缓冲液,运行电压20 kV,重力进样5 s(高度15 cm)。结果 25～400μg.mL-1羟苯乙酯线性关系良好,平均回收率97.9%,RSD=1.3%。结论所用方法准确、可靠且简便、易行。