建立了超高效液相色谱-串联质谱检测枳实药材中辛弗林、N-甲基酪胺的方法。以甲醇为提取溶剂,经QuECHERS分散净化,采用资生堂CAPCELL PAK CR色谱柱(150mm×2.0mm,5μm;C_(18)和SCX比例为1∶4)分离,质谱以正离子扫描,反应监测模式测...建立了超高效液相色谱-串联质谱检测枳实药材中辛弗林、N-甲基酪胺的方法。以甲醇为提取溶剂,经QuECHERS分散净化,采用资生堂CAPCELL PAK CR色谱柱(150mm×2.0mm,5μm;C_(18)和SCX比例为1∶4)分离,质谱以正离子扫描,反应监测模式测定。辛弗林和N-甲基酪胺在10~2000ng/mL范围内线性关系良好(R^(2)>0.997),检出限和定量限分别为0.3ng/mL和1.0ng/mL,回收率范围为94.3%~105.7%,相对标准偏差(RSD)均小于3%。该方法避免了使用磷酸盐和离子对试剂,仅在流动相中添加甲酸和甲酸铵,分析物就能有较好的保留,具有极高的质谱响应。相较于传统方法,该方法分析时间短、操作简单、专属性强,在强极性生物碱分离检测方面具有较好的应用价值。展开更多
A column chromatographic method has been developed for the separation and determination of cerium(Ⅲ) using poly[dibenzo-18-crown-6].The separation was carried out in L-valine medium.The adsorption of cerium(Ⅲ) was q...A column chromatographic method has been developed for the separation and determination of cerium(Ⅲ) using poly[dibenzo-18-crown-6].The separation was carried out in L-valine medium.The adsorption of cerium(Ⅲ) was quantitative from 1×10-1 to 1×10-4 mol/L L-valine.Amongst the various eluents,1.0-8.0 mol/L hydrochloric acid,1.0-8.0 mol/L hydrobromic acid,1.0-8.0 mol/L perchloric acid,1.0-2.0 mol/L sulfuric acid and 4.0-5.0 mol/L acetic acid,were found to be the efficient eluents for cerium(Ⅲ).The capacity of poly[dibenzo-18-crown-6] for cerium(Ⅲ) was(0.428±0.01) mmol/g.The method was applied to the separation of cerium(Ⅲ) from associated elements link uranium(Ⅵ) and thorium(Ⅳ).It was also applied for the determination of cerium(Ⅲ) in geological samples.The method is simple,rapid and selective with good reproducibility(approximately±2%).展开更多
A simple and selective method for the separation of Be（Ⅱ） was developed using poly[dibenzo-18-crown-6] as a stationary phase in column chromatography. The study was carried out in L-arginine medium. 1.0-8.0 M HCl a...A simple and selective method for the separation of Be（Ⅱ） was developed using poly[dibenzo-18-crown-6] as a stationary phase in column chromatography. The study was carried out in L-arginine medium. 1.0-8.0 M HCl and CH3COOH, 0.5-8.0 M HBr, HClO4 and H2SO4, 0.2-1.0 M EDTA and 0.02-0.12 M ammonium oxalate were found to be an efficient eluents for Be（Ⅱ）. The capacity of polymer was 0.554-0.01 mmol/g of crown polymer. The tolerance limit of various cations and anions were reported. Be（Ⅱ） was quantitatively separated from Mg（Ⅱ）, Ca（Ⅱ）, Sr（Ⅱ） and Ba（Ⅱ）. The selective separation of Be（Ⅱ） was possible from multicomponent mixtures. The method was extended to determine Be（Ⅱ） from geological samples. Method was simple, rapid and selective having good reproducibility （approximately4-2%）.展开更多
文摘建立了超高效液相色谱-串联质谱检测枳实药材中辛弗林、N-甲基酪胺的方法。以甲醇为提取溶剂,经QuECHERS分散净化,采用资生堂CAPCELL PAK CR色谱柱(150mm×2.0mm,5μm;C_(18)和SCX比例为1∶4)分离,质谱以正离子扫描,反应监测模式测定。辛弗林和N-甲基酪胺在10~2000ng/mL范围内线性关系良好(R^(2)>0.997),检出限和定量限分别为0.3ng/mL和1.0ng/mL,回收率范围为94.3%~105.7%,相对标准偏差(RSD)均小于3%。该方法避免了使用磷酸盐和离子对试剂,仅在流动相中添加甲酸和甲酸铵,分析物就能有较好的保留,具有极高的质谱响应。相较于传统方法,该方法分析时间短、操作简单、专属性强,在强极性生物碱分离检测方面具有较好的应用价值。
基金This work was supported by the University Grant Commission for awarding Junior Research Fellowship.
文摘A column chromatographic method has been developed for the separation and determination of cerium(Ⅲ) using poly[dibenzo-18-crown-6].The separation was carried out in L-valine medium.The adsorption of cerium(Ⅲ) was quantitative from 1×10-1 to 1×10-4 mol/L L-valine.Amongst the various eluents,1.0-8.0 mol/L hydrochloric acid,1.0-8.0 mol/L hydrobromic acid,1.0-8.0 mol/L perchloric acid,1.0-2.0 mol/L sulfuric acid and 4.0-5.0 mol/L acetic acid,were found to be the efficient eluents for cerium(Ⅲ).The capacity of poly[dibenzo-18-crown-6] for cerium(Ⅲ) was(0.428±0.01) mmol/g.The method was applied to the separation of cerium(Ⅲ) from associated elements link uranium(Ⅵ) and thorium(Ⅳ).It was also applied for the determination of cerium(Ⅲ) in geological samples.The method is simple,rapid and selective with good reproducibility(approximately±2%).
文摘A simple and selective method for the separation of Be（Ⅱ） was developed using poly[dibenzo-18-crown-6] as a stationary phase in column chromatography. The study was carried out in L-arginine medium. 1.0-8.0 M HCl and CH3COOH, 0.5-8.0 M HBr, HClO4 and H2SO4, 0.2-1.0 M EDTA and 0.02-0.12 M ammonium oxalate were found to be an efficient eluents for Be（Ⅱ）. The capacity of polymer was 0.554-0.01 mmol/g of crown polymer. The tolerance limit of various cations and anions were reported. Be（Ⅱ） was quantitatively separated from Mg（Ⅱ）, Ca（Ⅱ）, Sr（Ⅱ） and Ba（Ⅱ）. The selective separation of Be（Ⅱ） was possible from multicomponent mixtures. The method was extended to determine Be（Ⅱ） from geological samples. Method was simple, rapid and selective having good reproducibility （approximately4-2%）.
