Development of effective chromatographic or electrophoretic separation involves judicious deciding of selection of optimal experimental conditions that can provide an adequate resolution at a reasonable run time for t...Development of effective chromatographic or electrophoretic separation involves judicious deciding of selection of optimal experimental conditions that can provide an adequate resolution at a reasonable run time for the separation of interested components. Box-Behnken factorial design was effectively applied for the separation optimization of eight structurally related sulfonamides using capillary zone electrophorosis and reverse high performance liquid chromatography. Optimum values for volume ratio of THF to H2O in eluent, column temperature and flow rate of eluent are found as 12 to 88, 35℃ and 1.0 mL/min, respectively. Box-Behnken modified optimization model is extended to separation by capillary electrophoresis (CE). While using CE, a satisfactory separation is achieved with a minimum resolution larger than 1.0 for a separation time less than 10 min.展开更多
Uniform design was used to optimize extraction condition of direct refluence extraction of coumarins from the Chinese traditional medicine of radix angelicae pubescentis(Duhuo); the sum peak area of coumarins separate...Uniform design was used to optimize extraction condition of direct refluence extraction of coumarins from the Chinese traditional medicine of radix angelicae pubescentis(Duhuo); the sum peak area of coumarins separated with high performance liquid chromatography(HPLC) at detection wavelength of 320nm was considered as detection index, two factors of solvent concentration and extraction time were mainly studied at extraction temperature of 85℃ and a volume ratio of solvent to sample of 10∶1. Optimal subclass, quadric polynomial step by step aggression and neural network method were applied to process the experimental results. The results show that the first and second methods give the same factors combination (concentration of ethanol: 95%, extraction time: 3.6 h) and the second method is much better than the first one. The extraction model is consequently developed.展开更多
由于新型苯二氮[艹卓]类策划药物具有用量小、药效强、体内代谢快和含量低等特点,很难在受害人的血液和尿液中检出,而毛发具有检出时效长、易获取和易保存的优势,因此提出了题示方法.取剪至1~2 mm的毛发20 mg,加入1 m L含内标(1μg.L^(...由于新型苯二氮[艹卓]类策划药物具有用量小、药效强、体内代谢快和含量低等特点,很难在受害人的血液和尿液中检出,而毛发具有检出时效长、易获取和易保存的优势,因此提出了题示方法.取剪至1~2 mm的毛发20 mg,加入1 m L含内标(1μg.L^(-1)阿普唑仑Gd5)提取剂,于-50℃预冷5min,冷冻研磨两次,每次90s,中间间隔60s,并离心5min,取上清液浓缩至干,用100μL甲醇复溶,经0.22μm有机滤膜过滤.滤液在Acquity UPLCHSST3色谱柱上进行分离,经不同体积比的0.1%(体积分数,下同)甲酸溶液G含0.1%甲酸的乙腈溶液的混合液为流动相进行梯度洗脱,采用电喷雾离子源正离子模式(ESI+)扫描,多反应监测(MRM)模式检测,以保留时间和特征离子定性,内标法定量.结果表明,7种新型苯二氮[艹卓]类策划药物(瑞马唑仑、科纳唑仑、氟阿普唑仑、氟溴唑仑、玻玛唑仑、依替唑仑、溴替唑仑)工作曲线的线性范围为1~500pg.mg^(-1),检出限(3S/N)为0.11~0.35pg.mg^(-1).按照标准加入法进行回收试验,回收率为90.2%~104%,日内精密度和日间精密度试验所得相对峰面积的相对标准偏差(n=6)分别为1.7%~4.7%和2.9%~7.0%.展开更多
基金Project(20235010) support by the NSFC-KOSEF Scientific Cooperation ProgramProject supported by the Program for New Century Talents of University in Henan ProvinceProgram for Backbone Teacher in Henan Province, China
文摘Development of effective chromatographic or electrophoretic separation involves judicious deciding of selection of optimal experimental conditions that can provide an adequate resolution at a reasonable run time for the separation of interested components. Box-Behnken factorial design was effectively applied for the separation optimization of eight structurally related sulfonamides using capillary zone electrophorosis and reverse high performance liquid chromatography. Optimum values for volume ratio of THF to H2O in eluent, column temperature and flow rate of eluent are found as 12 to 88, 35℃ and 1.0 mL/min, respectively. Box-Behnken modified optimization model is extended to separation by capillary electrophoresis (CE). While using CE, a satisfactory separation is achieved with a minimum resolution larger than 1.0 for a separation time less than 10 min.
基金Project(2004714) supported by the Development and Innovation Committee of Hunan Province
文摘Uniform design was used to optimize extraction condition of direct refluence extraction of coumarins from the Chinese traditional medicine of radix angelicae pubescentis(Duhuo); the sum peak area of coumarins separated with high performance liquid chromatography(HPLC) at detection wavelength of 320nm was considered as detection index, two factors of solvent concentration and extraction time were mainly studied at extraction temperature of 85℃ and a volume ratio of solvent to sample of 10∶1. Optimal subclass, quadric polynomial step by step aggression and neural network method were applied to process the experimental results. The results show that the first and second methods give the same factors combination (concentration of ethanol: 95%, extraction time: 3.6 h) and the second method is much better than the first one. The extraction model is consequently developed.
