毛细管区带电泳法测定卷烟中的生物碱

在磷酸缓冲体系中采用毛细管区带电泳法测定卷烟中的生物碱时,检测灵敏度低,分离度差。考察了卷烟中生物碱的 提取条件,分离缓冲溶液的类型、pH值和浓度,卷烟中生物碱测定方法的线性范围、检出限、重现性和回收率。结果发 现,当采用410 mmol/L的酒石酸溶液（pH 2.8）为缓冲体系时,卷烟中生物碱的检测灵敏度和分离度均有明显改善,烟碱 的线性范围为0.06~0.80 mg/L（其他生物碱为0.006~0.10 mg/L）,检出限为0.002~0.01 mg/L,相对标准偏差为2.2%~10%,回收率为87.6%~102%。     

Cloud point extraction combined with micellar electrokinetic capillary chromatography determination of benzophenones in cosmetic matrix

A method has been developed for the separation and determination of three hydrophobic benzophenones: 2,4-dihydroxybenzophenone (BP-1), 2,2'4,4'-tetrahydroxybenzophenone (BP-2), and 2-hydroxy-4-methoxybenzophenone (BP-3) in sunscreen by micellar electrokinetic capillary chromatography (MEKC) combined with cloud point extraction (CPE). The analytes were extracted at pH 5.0 by micelles of the nonionic surfactant polyoxyethylene-7.5-octylphenyl ether (Triton X-114). A 150 microL aliquot from the extracted surfactant-rich phase was diluted up to 500 microL with ethanol to reduce its viscosity before separation by MEKC. A background electrolyte of 25 mmol/L sodium tetraborate containing 30 mmol/L sodium dodecyl sulfate at pH 9.25 was used as the separation medium to avoid the adsorption of hydrophobic substances and Triton X-114 onto the inner surface of the separation capillary, ensuring the separation efficiency and reproducibility. Detection is performed at 290 nm. Under the optimized conditions, an enrichment factor of 20 was obtained and the determination limits of BP-1, BP-2, and BP-3 were found to be 3.90 x 10(-) (7), 3.83 x 10(-7), and 6.42 x 10(-8) mol/L, respectively. In comparison with the earlier reported methods, the LODs of this method are superior to the other methods. The presented procedure was successfully applied to the determination of BP-1, BP-2, and BP-3 in sunscreen with satisfactory results.     

MECC分离并测定高粱及玉米中7种农药类环境激素

用毛细管胶束电动色谱成功分离并测定了高粱和玉米中7种农药类环境激素(多菌灵、西玛津、莠去津、毒死蜱、溴氰菊酯、乙草胺和氯氰菊酯)的残留量。研究了电泳缓冲液及表面活性剂等因素的影响,在最佳分离条件(pH 9.0、20 mmol/L磷酸氢二钠+50 mmol/L SDS+5%乙腈为缓冲溶液,分离电压20 kV,检测波长222 nm,实验温度25℃,压力法进样,30 mbar×10 s)下,7种农药在28 min内得到基线分离,质量浓度与其峰面积在5.0～150μg.L-1范围内呈良好线性,检出限为0.6～3.0μg/L,回收率为97%～108%,相对标准偏差为2.2%～4.7%。该方法具有操作简单、快速方便及自动化程度高、重现性好等优点。     

大体积进样-乙腈盐堆积-胶束扫集毛细管电动色谱法对马来酸氯苯那敏的测定

建立了大体积进样-乙腈盐堆积-胶束扫集毛细管电动色谱法测定马来酸氯苯那敏片中马来酸氯苯那敏的新方法,并考察了样品中乙腈和NaCl浓度对分离效果的影响.结果表明,以12 mmol/L四硼酸钠-50 mmol/L硼酸- 50 mmol/L十二烷基硫酸钠(SDS)为缓冲液(含10%甲醇,pH9.1),以70%乙腈- 200m...     

根际土壤溶液中磷的毛细管电泳分析

应用毛细管区带电泳间接紫外吸收法,对测定根际土壤溶液中PO43-的检测波长、电泳温度、分离电压和电解液组成等参数进行了选择,发展了根际土壤溶液中PO34-浓度的毛细管电泳分析法。选择后的电泳条件为:电解液为32mmol/L三羟甲基氨基甲烷+4mmol/L1,2,4-苯三酸+0.3mmol/L十六烷基三甲基溴化铵(pH=8.5);检测波长为205nm,分离电压为-20kV,温度为25℃。本方法有效地屏蔽了土壤溶液中Cl-,SO42-和NO3-等离子对PO43-测定的影响,对根际土壤溶液中PO43-的检出限为0.68mg/L(S/N=3);回收率为87.2%～99.4%,适于测定微量根际土壤溶液样品中PO34-的浓度。     

基于离子液体促进的手性配体交换毛细管电泳法分离分析去氧肾上腺素光学异构体

基于非手性离子液体对手性配体交换的促进作用,建立了一种测定去氧肾上腺素手性异构体的毛细管电泳分离分析方法。在系统优化了电泳条件后,采用20 kV的分离电压、25 ℃的毛细管柱温、254 nm的检测波长以及5 s的压力(3447 Pa)进样时间,在添加4.0 mmol/L Cu(Ⅱ)、8.0 mmol/L L-脯氨酸(L-Pro)和15 mmol/L氯化-1-丁基-3-甲基咪唑([BMIM]Cl)的20 mmol/L Tris-H₃PO₄缓冲溶液(pH 5.4)中,R-去氧肾上腺素和S-去氧肾上腺素的分离度为1.42,峰面积与质量浓度分别在12.5~150.0 mg/L和15.0~150.0 mg/L范围内有线性关系。将该方法用于加标血液和尿液样品中R和S型去氧肾上腺素的测定,尿液中的加标回收率为93.7%~108.2%,相对标准偏差在3.18%(n=3)以内;血液中的加标回收率为91.4%~113.1%,相对标准偏差在4.82%(n=3)以内。     

毛细管电泳-安培检测法用于7-甲基鸟苷与丝裂霉素C分离检测的研究

建立了一种同时分离检测7-甲基鸟苷与丝裂霉素C的毛细管电泳-安培检测方法。在950 mV电极(工作电极:0.3 mm微型石墨圆盘电极;参比电极:Ag/AgCl;辅助电极:Pt丝)电位下,于20 mmol/L的磷酸盐缓冲体系(pH 9.4)中,采用18 kV的分离电压进行分离。在最佳条件下,7-甲基鸟苷与丝裂霉素C在10 min内实现分离,7-甲基鸟苷与丝裂霉素C的线性范围均为0.50~50 mg/L,检测限分别为0.050 mg/L与0.025 mg/L。将该方法用于模拟尿样和模拟兔血清样的检测,7-甲基鸟苷与丝裂霉素C的回收率为93.0%～97.2%,结果令人满意。     

黑火药余烬中无机阴离子的毛细管电泳方法研究

 发展了一种用于黑火药余烬中无机阴离子测定的毛细管电泳分析方法。对缓冲溶液的组成及pH值、电渗流改性剂的浓度以及分离电压等条件进行了研究。选定条件 :分离电压为 - 2 0kV ,缓冲溶液为 5 0mmol/L的Na2 CrO4(pH 8 2 0 ) ,电渗流改性剂为 0 5mmol/L的溴化十六烷基三甲基铵 (CTAB) ,检测波长为 2 5 4nm。在上述条件下 ,5种阴离子在 4min内可完全分离。各组分迁移时间和峰面积的相对标准偏差 (RSD)分别为 0 17%～1 4 0 %和 3 9%～ 5 0 % ,最低检测限为 5 0 μmol/L～ 10 0 μmol/L。     

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。     

Analysis of organic acids and inorganic anions in beverage drinks by capillary electrophoresis

To meet the need for a new and validated analytical method for simultaneous determination of inorganic and organic acid anions in beverage drinks, a capillary zone electrophoresis (CZE) procedure had been developed based on a new background electrolyte (BGE) system containing 3 mmol/L 1,3,5-benzenetricarboxylic acid (BTA), 15 mmol/L tris(hydroxymethyl)aminomethane and 1.5 mmol/L tetraethylenepentamine (TEPA) at pH 8.4. Baseline separation of anions commonly found in beverage drinks could be achieved in less than 14 min with indirect UV detection at 240 nm. Comigration problems for hydroxycarboxylic acids could be solved using TEPA as BGE additive. The results indicate excellent repeatability for migration time (RSD, 0.27-0.67%, n = 5) and good precision for both peak height (RSD, 3.2-4.2%, n = 5) and peak area (RSD, 3.1-4.5%, n = 5). Under the optimized conditions and using corrected peak area for quantitation, an excellent linear dynamic range (with correlation coefficient > 0.997 in a concentration range from 0.005 to 2.0 mmol/L) and low detection limit (1-4 micro mol/L) were obtained for all the anions investigated. The applicability and reliability of the CE procedure developed were established by parallel method determination using established ion chromatography procedure for the analysis of inorganic and organic acid anions in orange juice and wine samples. Our CZE procedure provided a sensitive and economic technique for simultaneous determination of inorganic and organic acid anions in orange juice, red and white wine samples.     

双丙酮-D-甘露糖醇—硼酸络合酸手性毛细管电泳法分离盐酸莱克多巴胺立体异构体

采用手性多羟基化合物—硼酸络合酸为手性选择剂,建立了分离盐酸莱克多巴胺4个立体异构体的手性毛细管电泳(NACE)方法.实验考察了手性选择剂的种类、浓度和三乙胺浓度对手性分离效果的影响.结果表明,双丙酮-D-甘露糖醇—硼酸络合酸手性选择剂的分离效果最好,优化的缓冲溶液组成为含100 mmol/L双丙酮-D-甘露糖醇、10...     

Effects of electrolyte modification and capillary coating on separation of glycoprotein isoforms by capillary electrophoresis

The capillary electrophoresis (CE) running electrolyte composition was optimized for the separation of selected glycoproteins. A good separation of the ovalbumin (OV) and alpha-acid glycoprotein (AAG) isoforms was achieved in 20 mmol x L(-1) N-(2-hydroxyethyl)piperazine-2'-(2-ethanesulfonic acid) (HEPES) at pH 7.0, in 20 mmol x L(-1) phosphate, pH 7.0, or in 25 mmol x L(-1) borate, pH 7.9. Various ways of suppression of the glycoprotein adsorption onto the capillary wall were compared. Alpha, omega-diamine alkanes and bis(aminoalkyl) amines were added to the CE buffers, the optimized concentration being 1 mmol x L(-1) in 20 mmol x L(-1) phosphate buffer. The OV and AAG isoforms could be separated using all the alpha,omega-diamine alkanes or bis(2-aminoethyl)amine. The length of the alkyl chain in the diaminoalkane did not influence the separation. The separation of the isoforms of pollen allergens was also tested. The effects of modification of the capillary wall by succinyl-poly-L-lysine and hydrophilic CElect-P1 capillary were compared. A decrease in the glycoprotein and protein adsorption resulted in an improved separation of the isoforms.     

托吡卡胺对映体的毛细管电泳-方波安培分离检测

采用毛细管电泳-方波安培检测法,在熔融石英毛细管(75 μm i.d.×50 cm)中,以7 mmol/L 三羟甲基氨基甲烷(Tris)-10 mmol/L柠檬酸-2 mmol/L硼酸-15mmol/L β-环糊精 （β-CD） (pH 3.0)为电泳介质,采用重力进样,高度差为20 cm,进样时间为10 s,在分离电压为15 kV,方波平衡电位+0.8 V的条件下,实现了托吡卡胺对映体的分离检测。线性范围为5~750 μmol/L,检出限为2 μmol/L。对影响分离度的因素β-CD浓度、硼酸浓度及p     

电堆积在线扫集胶束电动色谱法测定苦参中的生物碱

建立了电堆积在线扫集胶束电动色谱法测定苦参碱和槐定碱的新方法.考察了pH值、磷酸二氢钠浓度、CTAB浓度、电压、有机溶剂和进样时间对分离效果的影响.采用未涂层熔融石英毛细管,以20mmol/L磷酸二氢钠-0.8 mmol/L CTAB-100mmol/L Tris(含10%异丙醇,pH 8.9)为缓冲液,在进样电压-1...     

连花清瘟胶囊中6种有效成分的毛细管胶束电动色谱法测定

建立了毛细管胶束电动色谱法同时测定中药复方制剂连花清瘟胶囊中甘草苷、芦丁、金丝桃苷、槲皮苷、绿原酸、大黄酸6种药效成分含量的分析方法.使用未涂层弹性石英毛细管,以50 mmol/L SDS-15mmol/L磷酸氢二钠-15 mmol/L硼酸(含25%异丙醇,pH=8.0)作电解质,于254 nm下紫外检测,被测组分在3...     

Capillary electrophoresis coupled with electrochemical detection using porous etched joint for determination of antioxidants

Capillary electrophoresis coupled with electrochemical detection (CE-EC) for determination of antioxidants, propyl gallate (PG) and tert-butylhydroquinone (TBHQ), in cosmetic samples was proposed in this work. A porous etched joint was used to isolate the electrochemical detection from the electrophoretic high voltage. Compared with the 25 microm i.d. capillary without a decoupler in a CE-EC system, a 75 microm i.d. capillary applied in the present system gave an improvement in both sample injection and sensitivity. Moreover, the carbon fiber working electrode could be directly in touch with the end of separation capillary due to the elimination of the effect of separation voltage on the EC detection, so the alignment of working electrode and capillary became easy and the dead volume was also decreased. Baseline separation of the two antioxidants was achieved by CE in a 50 cm long x 75 microm i.d. capillary at 20 kV using 5.0 mmol L(-1) phosphate buffer (pH 8.00). 0.7 V (versus Ag/AgCl) was applied to the carbon fiber electrode for electrochemical detection. Under the optimal condition, the precisions (RSD, n=4) of peak height and migration time of PG and TBHQ were 2.39-3.59% and 0.34-0.44%, respectively. The detection limits of PG and TBHQ were 2.51x10(-6) and 4.88 x 10(-6) mol L(-1) for standard solution and 0.0751 and 0.0328 mg g(-1) for the real cosmetic samples with consumption of 0.3g sample. Analysis of TBHQ and PG in cosmetics samples was also achieved with the present system and the spiked recoveries of two analytes in cosmetics samples were in the range of 93.6-98.8%.     

固相萃取-离子色谱法测定地下水中痕量高氯酸根离子

建立了测定地下水中痕量高氯酸根（ClO~4）的固相萃取-离子色谱(SPE-IC)分析方法。0.7 L水样经预处理降低主要干扰离子Cl~、CO2~3和SO2~4的干扰后,使用Cleanert PWAX弱阴离子交换固相萃取小柱对地下水中痕量(μg/L级)的ClO~4进行富集,用6 mL 1%NaOH溶液洗脱,富集液经0.45 μm水膜过滤后,用IonPac AS20阴离子分离柱、50 μL进样环、40 mmol/L KOH溶液淋洗、抑制电导检测分离分析。结果表明,地下水样品中ClO~4的方法检出限和测定下限分别为0.15 μg/L和0.60 μg/L,进样质量浓度在1～15 μg/L范围内有很好的线性关系,线性相关系数为0.9992,回收率为99.7%～100.5%;该方法经济有效,可用于地下水中痕量ClO~4的检测。利用该方法测定了哈尔滨周边部分地区地下水中ClO~4浓度,检测结果与离子色谱-质谱联用法的检测结果的相对误差为1.85%～9.24%。     

High-performance capillary zone electrophoretic assay for markers of diabetic nephropathy in plasma and urine

A new high-performance capillary zone electrophoretic assay for creatine (Cr), creatinine (Cn), urea (U) and uric acid (Ua), markers of human diabetic nephropathy, both in plasma and urine has been developed with UV detection at 200 nm. The plasma sample was deproteinized with trichloroacetic acid and centrifuged at 10 000 rpm for 10 min. The urine sample was diluted 20-fold with buffer before analysis. The optimum separation conditions for the markers was investigated with respect to the concentration of the buffer, the pH, the voltage and the capillary temperature. Baseline separation was achieved in 25 mmol/L phosphate buffer (pH 3.45) using a 21 cm x 75 microm I.D. fused-silica capillary at 40 degrees C with an electric field of 1190 V/cm. The calibration curves showed good linearity in the range 3.5-1000, 0.18-700, 500-5000 and 2-800 microM (r2 min > 0.998) for Cr, Cn, U and Ua, respectively. The proposed method also has a high reproducibility (peak area RSD max < 3%) and has been successfully applied to the determination of clinical samples.     

在线扫集-胶束毛细管电动色谱法测定复方氨酚烷胺胶囊中的3种有效成分

以在线扫集-胶束毛细管电动色谱法(Sweeping-MEKC)测定了复方氨酚烷胺胶囊中的马来酸氯苯那敏、咖啡因和对乙酰氨基酚3种有效成分。考察了缓冲溶液pH值、SDS浓度、分离电压及进样时间等对分离效果的影响。优化条件:以未涂层熔融石英毛细管(55 cm×50μm,有效柱长35 cm)为分离柱;环境温度25℃;80 mmol/L十二烷基磺酸钠+20 mmol/L NaH2PO4(pH 2.2)+15%乙腈为缓冲体系,分离电压-20kV,进样时间60 s(H=20.0 cm),测量波长210 nm。在该条件下氯苯那敏、咖啡因和对乙酰氨基酚在25min内出峰,峰面积RSD均小于4%;线性范围分别为2.45～39.17、1.61～25.76、1.58～25.28 mg/L;检出限(S/N=3)分别达139、34、24μg/L,回收率分别为96%～101%、98%～102%、96%～102%。     

毛细管区带电泳-间接紫外检测法快速测定食品中乳糖、蔗糖、葡萄糖和果糖

建立了毛细管区带电泳-间接紫外检测快速测定食品中乳糖、蔗糖、葡萄糖和果糖的方法。以水或5 mmol/L醋酸为样品提取液,未涂层熔融石英毛细管(30.2 cm(有效长度20 cm)×50 μm)为分离柱,4 mmol/L山梨酸钾+10 mmol/L磷酸钠+30 mmol/L NaOH(pH 12.56)+0.5 mmol/L十六烷基三甲基溴化铵(CTAB)为分离缓冲液,在-8 kV下分离,于254 nm波长下检测,10 min内实现了食品中上述4种糖的同时分离与测定。乳糖、蔗糖、葡萄糖和果糖的检出限(S/N=3)分别为50、75、25和25 mg/L,定量限(S/N=10)分别为150、225、75和75 mg/L,回收率在87.0%~107.0%之间,相对标准偏差在1.2%~4.7%之间。整个实验过程未使用有机溶剂。用该法测定了9种食品样品及1个质控样品,结果表明该法简单、快速、准确,适用于食品中乳糖、蔗糖、葡萄糖和果糖的日常测定。