胶束电动毛细管色谱法测定牡丹皮及六味地黄丸中丹皮酚的含量

目的用胶束电动毛细管色谱法分离测定中药材牡丹皮及中成药六味地黄丸中丹皮酚的含量。方法定量采用内标法 ,选取芦丁为内标。所用毛细管规格为 5 5cm(有效长度 5 0cm)× 75 μm,检测波长 2 74nm ,电压 1 5kV ,背景电解质分别为 30mmol/LSDS -30mmol/L硼砂 ,2 0mmol/LSDS -5 0mmol/L硼砂 ( pH 9 4 )。 结果线性分别为 6～ 4 2mg/L,1 8 2～ 91mg/L;相关系数分别为0 9995和 0 9997;RSD为 1 95 %和 3 6 %;加样回收率为 1 0 1 5 %～ 1 0 3 3%和 97 7%～1 0 1 9%。丹皮酚含量分别为 1 5 9%和 0 1 4 8%。结论胶束电动毛细管色谱法用于测定牡丹皮及六味地黄丸中丹皮酚的含量是可行的。     

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.     

Simultaneous determination of flavonoids in Ixeridium gracile by micellar electrokinetic chromatography

A micellar electrokinetic chromatography (MEKC) method has been developed for the quantitative analysis of five flavonoids: luteolin 7-O-glucoside (LG), 2′,4′-dihydroxy-dihydrochalcone (DD), 2′,4′-dihydroxy-chalcone (DC), 7-hydroxy-flavanone (HF) and quercetin 3-O-galactoside (QG) in Ixeridium gracile with UV detection at 275 nm. The applied voltage was 25 kV and the capillary temperature was kept constant at 25 °C. The effects of buffer pH, the concentration of electrolyte and organic modifier on migration behavior were studied. Optimum separation condition was achieved with 15 mM borate, 30 mM sodium dodecyl sulfate (SDS) and 10% (v/v) ethanol at pH 10.5. Regression equations showed good linear relationships (correlation coefficients: 0.9984, 0.9991, 0.9994, 0.9995 and 0.9997) between the peak area of each compound and their concentrations. The relative standard deviations (R.S.D.) of the migration time and peak area were less 1.67 and 3.53% (intra-day), and 1.82 and 3.73% (inter-day), respectively, under the optimum separation conditions. The contents of the five active compounds in I. gracile were determined with satisfactory repeatability and recovery.     

用毛细管电泳法测定喘咳宁片中盐酸麻黄碱和巴比妥的含量

用毛细管区带电泳法同时测定喘咳宁片中的盐酸麻黄碱和巴比妥的含量 .以苯巴比妥为内标物 ,以 2 0mmol/L硼砂 2 0mmol/L磷酸二氢钠 (pH 7.0 )为运行缓冲液 ,分离电压为 9.0kV时 ,在 9min内完成分离 .盐酸麻黄碱和巴比妥分别在 0 .17～ 1.39mmol/L和 0 .5 4～ 4.16mmol/L范围内有良好线性关系 (r =0 .9987和r =0 .996 3) ,最低检测限分别为 2 .97μmol/L和3.2 6 μmol/L(S/N >3) ,回收率分别为 99.4%和 10 2 .2 % ,系统的精密度良好 ,RSD在 5 .0 %以内 .     

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。     

MECC determination of oleanolic acid and ursolic acid isomers in Ligustrum lucidum Ait

In this paper, a novel method to separate and determine oleanolic acid and ursolic acid isomers in Ligustrum lucidum Ait was studied by micellar electrokinetic capillary chromatography (MECC). The baseline separation of the two analytes were obtained on the condition that the buffer contained 15 mmol/l disodium hydrogen phosphate, 15 mmol/l disodium tetreborate, 10 mmol/l SDS and 5% (v/v) alcohol. The contents of the oleanolic acid and ursolic acid were determined in L. lucidum Ait, Folium photiniae and Flos campsis; they were 78.3 (R.S.D. = 2.75%) and 20.7 mg/g (R.S.D. = 2.97%), 27.9 (R.S.D. = 3.67%) and 79.8 mg/g (R.S.D. = 3.44%), 65.5 (R.S.D. = 3.73%) and 60.4 mg/g (R.S.D. = 4.06%) (n = 5), respectively. The recoveries of the analytes in the extract of L. lucidum Ait were 102%, (R.S.D. = 2.85%) for oleanolic acid and 104% (R.S.D. = 3.21%) for ursolic acid (n = 5). With the emphasis on the effects of SDS and alcohol concentrations on the separation of the isomers were investigated.     

Separation and determination of coumarins in the root bark of three citrus plants by micellar electrokinetic capillary chromatography

A micellar electrokinetic capillary chromatography (MEKC) method for the determination of xanthyletin and xanthoxyletin in the roots bark of three Citrus plants was developed for the first time. The electrophoresis buffer was 10 mmol/L sodium borate containing 50 mmol/L sodium dodecyl sulfate, 20% (v/v) acetonitrile and 10 % (v/v) methanol (pH 9.8). The correlation coefficients of the calibration curves for xanthyletin and xanthoxyletin are 0.9993 and 0.9999, respectively, over the concentration ranges (16.0-800.0 mg/L; 8.0-400.0 mg/L).     

Determination of hydroxyanthraquinoids in Rhubarb by cyclodextrin-modified micellar electrokinetic chromatography using a mixed micellar system of sodium dodecyl sulfate and sodium cholate

A cyclodextrin-modified micellar electrokinetic chromatographic (CD-MEKC) method was established to determine five hydroxyanthraquinoids in Rhubarb. The five components were successfully separated by using the mixed micellar system consisting of 20 mmol/l sodium dodecyl sulfate (SDS) and 20 mmol/l sodium cholate (SC) with 10 mmol/l beta-cyclodextrin in phosphate buffer (pH 10.4). The separation was optimized by adjusting buffer pH, concentrations of beta-cyclodextrin and SC and applied voltage. The proposed method was validated and applied to the determination of two commercial Rhubarb samples. The results obtained were satisfactory.     

Simultaneous determination of iridoid glycosides and flavanoids in Lamionphlomis rotate and its herbal preparation by a simple and rapid capillary zone electrophoresis method

Iridoid glycosides and flavanoids are two main effective components of Lamiophlomis rotata (Benth.) kudo. However, there is no method for simultaneous analysis of iridoid glycosides and flavanoids in L. rotata and its pharmaceutical preparations. A simple and rapid capillary zone electrophoresis (CZE) method was developed and validated for simultaneous determination of two iridoid glycosides (8-O-acetylshanzhiside methylester and 8-deoxyshanzhiside) and three flavanoids (apigenin, quercetin and luteolin) in L. rotata. Operational variables, such as the voltage, buffer concentration and pH were optimized, the final optimum separation condition was 10 mM sodium tetraborate-20 mM NaH(2) PO(4) (pH 8.5)-15% (v/v) methanol, 238 nm UV detection, 18 kV applied voltage. The linearity and the recovery of the proposed method were very satisfactory (correlation coefficients were 0.9994-0.9998 and the recoveries were 94.5-108.8% for the analytes) and the method allowed analytes in real samples to be determined within 9 min. The proposed CZE method can be used for quality control of iridoid glycosides and flavanoids in L. rotata and its herbal preparation.     

毛细管区带电泳法测定山茱萸及六味地黄丸中没食子酸含量

目的用毛细管区带电泳法分离测定中药材山茱萸及中成药六味地黄丸中没食子酸的含量。方法定量采用内标法 ,选取肉桂酸为内标。所用毛细管规格为 60cm(有效长度 4 5cm)× 75 μm,检测波长 2 71nm ,电压 2 0kV ,背景电解质为 2 0mmol/L硼砂。结果线性范围为 1 5 6～ 3 1 2mg/L ,相关系数r =0 9993 (n =7) ,RSD分别为 2 9%和 2 1 % (n =5 ) ,加样回收率为 97 4 %～ 98 6%和 99 3 %～ 1 0 2 4 % ,没食子酸含量分别为 0 2 2 5 %和 0 0 5 5 %。结论毛细管区带电泳法用于测定山茱萸及中成药六味地黄丸中没食子酸的含量是可行的     

Chiral separation of pemoline enantiomers by cyclodextrin-modified micellar capillary chromatography

Micellar electrokinetic chromatography (MEKC) was successfully applied to the chiral separation with the addition of cyclodextrins (CDs) as chiral selector to running buffer. Chiral separation depended on the type of CDs. Mono-3-O-phenylcarbamoyl-beta-CD was effective for the chiral separation of pemoline. We investigated the type and concentration of CD and other parameters such as buffer pH, the concentration of SDS and the effect of organic modifier. The conditions for enantiomeric separation of pemoline were as follows: 40 mmol/l borate buffer at pH 9.0 with 40 mmol/l SDS, 20 mmol/l mono-3-O-phenylcarbamoyl-beta-CD and 10% 2-propanol. Baseline separation (Rs=2.21) of pemoline can be achieved.     

刺五加及其注射液中槲皮素的含量测定

目的 :建立高效毛细管电泳法测定刺五加和刺五加注射液中槲皮素的含量方法。方法 :运行缓冲液为50mmol/L硼酸 -50mmol/L十二烷基磺酸钠缓冲液 ,pH值为8 5 ,操作电压为20kV ,检测波长为260nm。结果 :测定槲皮素的线性范围为0 0125～1 0mg/ml ,r=0 9997 ;刺五加的加样回收率为 (98 99±0 63) % ,刺五加注射液的加样回收率为 (98 62±0 42) %。结论 :本分析方法简便、快速、准确 ,适合刺五加及刺五加注射液中槲皮素的含量测定     

Simultaneous determination of HIV-protease inhibitors lamivudine and zidovudine in pharmaceutical formulations by micellar electrokinetic chromatography

A micellar electrokinetic chromatographic (MEKC) method for the simultaneous separation and determination of lamivudine (LMV) and zidovudine (ZDV) in pharmaceutical formulation has been developed. Factors that affect the separation, such as buffer pH, surfactant concentration (sodium dodecyl sulfate, SDS), organic solvents and applied voltage were optimized. Buffer consisting of 12.5 mM sodium tetraborate decahydrate and 15 mM boric acid adjusted at pH 10.8, containing 90 mM SDS and 5% (v/v) acetonitrile (ACN) was found to be suitable for the separation of the drugs. p-Aminobenzoic acid (PABA) was used as internal standard (I.S.). Detection of analytes and I.S. was performed at a wavelength of 210 nm. It was observed that both the drugs and I.S. were migrated within 20 min at the applied voltage of +10 kV. Validation of the method was performed in terms of linearity, accuracy, precision, limit of detection (LOD) and quantification (LOQ). An excellent linearity was obtained in the concentration range 10-80 microg/ml for LMV and 10-100 microg/ml for ZDV. The detection limits for LMV and ZDV were found to be 2.5 and 2.0 microg/ml, respectively. The optimized method was applied to the simultaneous determination of LMV and ZDV in pharmaceutical formulation and human plasma (spiked) samples. Recovery of both the drugs in tablet dosage form and spiked drugs in plasma were > or =99.72% (relative standard deviation (R.S.D.)< or =1.84%) and > or =80.4% (R.S.D.< or =5.4%), respectively. In the electropherogram no interfering peaks were observed in the region of analytes and I.S. due to inactive ingredients in the tablets and matrices in plasma.     

Determination of kava lactones and flavonoid glycoside in Scorzonera austriaca by capillary zone electrophoresis

A capillary zone electrophoretic method has been developed for the quantitative analysis of three active comppounds, 12-hydroxy-desmethoxyyangonin (HD), 12-beta-d-glucopyranoside-desmethoxyyangonin (GD) and luteolin 3'-(6-E-p-coumaroyl-beta-d-glucopyranoside) (LG) in Scorzonera austriaca with UV detection at 254 nm. The applied voltage was 25 kV and the capillary temperature was kept constant at 25 degrees C. The effect of buffer pH, the concentration of electrolyte and organic modifier on migration were studied systematically. Optimum separation was achieved with 20 mM borate buffer at pH 10.00 containing 10% (v/v) methanol. Daphnetin was used as internal standard for quantification. Regression equations revealed good linear relationship between the ratios of the peak area of each compound and its the ratios of concentration. All the correlation coefficients were higher than 0.9990. The relative standard deviations of migration time and the peak area were <1.46% and 5.13% (inter-day), and <1.65% and 5.16% (intra-day), respectively. The contents of the three compounds in S. austriaca were successfully determined with satisfactory repeatability and recovery.     

Application of micellar electrokinetic chromatography for the separation of retinoids

The applicability of micellar electrokinetic chromatography (MEKC) using sodium dodecylsulphate (SDS) as pseudo-stationary phase for the separation of five retinoids (retinol, retinal, retinyl acetate, retinyl palmitate, retinoic acid), was investigated. The effects of the acetonitrile content, the SDS concentration, the pH and the addition of Brij 35 to the background electrolyte on the migration behaviour of the retinoids were determined. It was found that the effective mobilities of retinol, retinal and retinyl acetate could be easily regulated through the ACN content and the SDS concentration of the BGE. The electrophoretic behaviour of the very hydrophobic retinyl palmitate was abnormal. Under various conditions this compound showed up as a late, very sharp peak. A strong indication was found that the retinyl palmitate forms a stable, charged complex with SDS during sample preparation. The mobility of the retinyl palmitate peak could be regulated, independently from the other peaks, through the Brij concentration of the BGE. Using a running buffer consisting of Tris buffer (pH 8), 20 mmol l(-1) SDS, 1 mmol l(-1) Brij 35 and 35% (v/v) acetonitrile, a complete separation of the five retinoids could be realised in less than 20 min.     

毛细管电泳法测定一清颗粒中七种成分的含量

建立了毛细管电泳法测定一清颗粒中的7种有效成分--盐酸小檗碱、汉黄芩苷、汉黄芩素、大黄素、芦荟大黄素、大黄酚和大黄素甲醚.采用未涂层弹性融硅石英毛细管柱,盐酸小檗碱的测定:以盐酸雷尼替丁为内标,运行缓冲液为0.2 mol/L磷酸二氢钠溶液-无水乙醇(1:1,pH 5.5),分离电压21 kV,重力进样10 S(高度15 cm),检测波长265 nm.其他6组分的测定:以对乙酰氨基酚为内标,运行缓冲液为8%甲醇(pH 9.42,含25 mmol/L 硼砂、25 mmol/LSDS和4mmol/L磺丁基-β-环糊精),分离电压14 kV,重力进样5 s(高度15 cm),检测波长254 nm.7种成分分别在2.6～13、2～20、l～10、1.6～16、1.2～12、7.2～72和l～10 μg/ml浓度范围内线性关系良好,回收率分别为100.3%、102.7%、101.8%、102.0%、99.0%、100.0%、98.2%,脚均小于3.09%.     

高效毛细管电泳法测定葛根及其制剂正心泰胶囊中葛根素的含量

目的：测定葛根（野葛,粉葛）及其制剂正心泰胶囊中葛根素的含量。方法：采用高效毛细管电泳法,双氯灭痛为内标物。测定条件为：运行缓冲液：30mmol/L硼砂缓冲溶液（PH：9．37）,操作电压30kv,柴外检测波长254nm,结果：葛根素的线性范围为10－100ug/ml,葛根的平均回收率为97．53％（RSD：2．1％,=5),,正心泰胶囊平均回收率为：102．31%(RSD:1.7%,n=5),结论：该方法简便,快捷,具有良好的精密度,回收率和线性关系,结果满意。     

Determination of paeonol and paeoniflorin in Chinese medicine Cortex Moutan and 'Shuangdan' granule by micellar electrokinetic capillary chromatography

An easy, simple and rapid micellar electrokinetic capillary chromatography (MEKC) method was developed for the separation of two active components paeonol (PN) and paeoniflorin (PF) within 7 min. Capillary electrophoresis (CE) was performed using a 50.0 cm (42.0 cm to the detector window) ×75 μm i.d. fused-silica capillary. The optimal running buffer containing 10 mM borate and 25 mM SDS at pH 9.54 was employed. The applied voltage 15 kV and the temperature 25 °C was used in CE separation. The linearities between peak areas and the concentrations of the analytes were investigated, and they exhibited excellent linear behavior over the investigated concentration ranges (R²: 0.9945 for PN and 0.9992 for PF). The method was successfully applied to the determination of these two components contained in Cortex Moutan and ‘Shuangdan’ granule. The average recoveries ranged between 97.6 and 105.3% for PN and 95.3 and 106.1% for PF, respectively.     

Identification and determination of oligomeric stilbenes in the roots of Caragana species by capillary electrophoresis

A method based on capillary electrophoresis with electrochemical detection (CE-ED) was employed for the determination of one alkaloid (hypaphorine) and the four oligomeric stilbenes, pallidol, kobophenol A, miyabenol C and (+)-alpha-viniferin in the roots of Caragana species. The five analytes could be well separated within 12 min in a 40 cm length capillary at a separation voltage of 12 kV in a 100 mmol/L borate buffer (pH 10.0). The response was linear over about 3 orders of magnitude for all investigated analytes with detection limits (S/N = 3) ranging from 0.0385 to 0.111 mg/L. The five constituents presented in Caragana sinica can also be detected in the roots of other Caragana species, but their contents were quite different. It is demonstrated that CE-ED is a useful technique for the investigation of some electroactive constituents in plants.     

Determination of nateglinide in animal plasma by micellar electrokinetic chromatography and on-line sweeping technique

A micellar electrokinetic chromatography (MEKC) method was developed for the determination of nateglinide in animal plasma by on-line sweeping technique, in which plasma samples were simply deproteinized with acetonitrile, and analyzed with 16 mmol/L NaH2PO4 + 6 mmol/L Na2B4O7 + 60 mmol/L sodium dodecyl sulfate (SDS) (pH 7.14) as the running buffer, a fused-silica capillary as the separation tube, 21 kV as the running voltage and UV detection at 214 nm. Under these conditions, more than 100-fold enrichment of nateglinide was obtained with the good linear relation in the range of nateglinide plasma concentration 0.2-7 mg/L (R = 0.998). The method could be applied successfully to determine trace drugs in clinical analysis.