A novel analytical method was developed for determining morpholinium cations lacking ultraviolet absorption groups.This determination was carried out by high performance liquid chromatographyindirect ultraviolet(HPLC-...A novel analytical method was developed for determining morpholinium cations lacking ultraviolet absorption groups.This determination was carried out by high performance liquid chromatographyindirect ultraviolet(HPLC-1UV) detection using imidazolium ionic liquid as background absorption reagents,and imidazolium ionic liquid aq.soln.-organic solvent as mobile phase by a reversed-phase C18 column.The background ultraviolet absorption reagents,imidazolium ionic liquids and organic solvents were investigated.The imidazolium ionic liquid in the mobile phase is not only the background ultraviolet absorption reagent for IUV,but also an active component to improve the separation of morpholinium cations.It was found that morpholinium cations could be adequately determined when0.5 mmol/L 1-ethyl-3-methylimidazolium tetrafluoroborate aq.soln./methanol(80:20,v/v) was used as mobile phase with an IUV detection wavelength of 210 nm.In this study,the baseline separation of Nmethyl,ethylmorpholinium cations(MEMo) and N-methyl.propylmorpholinium cations(MPMo) was successfully achieved in 8.5 min.The detection limits(S/N = 3) for MEMo and MPMo were 0.15 and0.29 mg/L,respectively.This simple and practical method has been successfully applied to the determination of two morpholinium ionic liquids synthesized by the chemistry laboratory.展开更多
目的建立分散微固相萃取-高效液相色谱法测定荷丹片中荷叶碱、O-去甲基荷叶碱、N-去甲基荷叶碱的含量的新方法。方法以强离子交换树脂(PCX)为吸附剂,通过对DMSPE技术中PCX用量、吸附时间、洗脱溶剂氨-乙腈浓度和洗脱体积的优化,实现样...目的建立分散微固相萃取-高效液相色谱法测定荷丹片中荷叶碱、O-去甲基荷叶碱、N-去甲基荷叶碱的含量的新方法。方法以强离子交换树脂(PCX)为吸附剂,通过对DMSPE技术中PCX用量、吸附时间、洗脱溶剂氨-乙腈浓度和洗脱体积的优化,实现样品中荷叶碱的最优提取纯化。结果建立了测定荷丹片中荷叶碱、O-去甲基荷叶碱、N-去甲基荷叶碱含量的分散微固相萃取-高效液相色谱法,分散微固相萃取的最佳工艺条件为:PCX用量25 mg,涡旋30 s,以3.0 mL 5%的氨-乙腈溶液进行洗脱。结论建立的含量测定方法可用于荷丹片中荷叶碱、O-去甲基荷叶碱、N-去甲基荷叶碱含量的分析测定。该方法简单精确,稳定性高;样品处理快捷简便,溶剂损耗明显减少;设备要求低,装置简便;分析速度快,分析周期短。展开更多
基金supported by the Natural Science Foundation of Heilongjiang Province(No.B201307)the Ministry of Education of Heilongjiang Province(No.12531192)the Program for Scientific and Technological Innovation Team Construction in Universities of Heilongjiang Province(No.2011TD010)
文摘A novel analytical method was developed for determining morpholinium cations lacking ultraviolet absorption groups.This determination was carried out by high performance liquid chromatographyindirect ultraviolet(HPLC-1UV) detection using imidazolium ionic liquid as background absorption reagents,and imidazolium ionic liquid aq.soln.-organic solvent as mobile phase by a reversed-phase C18 column.The background ultraviolet absorption reagents,imidazolium ionic liquids and organic solvents were investigated.The imidazolium ionic liquid in the mobile phase is not only the background ultraviolet absorption reagent for IUV,but also an active component to improve the separation of morpholinium cations.It was found that morpholinium cations could be adequately determined when0.5 mmol/L 1-ethyl-3-methylimidazolium tetrafluoroborate aq.soln./methanol(80:20,v/v) was used as mobile phase with an IUV detection wavelength of 210 nm.In this study,the baseline separation of Nmethyl,ethylmorpholinium cations(MEMo) and N-methyl.propylmorpholinium cations(MPMo) was successfully achieved in 8.5 min.The detection limits(S/N = 3) for MEMo and MPMo were 0.15 and0.29 mg/L,respectively.This simple and practical method has been successfully applied to the determination of two morpholinium ionic liquids synthesized by the chemistry laboratory.
文摘目的建立分散微固相萃取-高效液相色谱法测定荷丹片中荷叶碱、O-去甲基荷叶碱、N-去甲基荷叶碱的含量的新方法。方法以强离子交换树脂(PCX)为吸附剂,通过对DMSPE技术中PCX用量、吸附时间、洗脱溶剂氨-乙腈浓度和洗脱体积的优化,实现样品中荷叶碱的最优提取纯化。结果建立了测定荷丹片中荷叶碱、O-去甲基荷叶碱、N-去甲基荷叶碱含量的分散微固相萃取-高效液相色谱法,分散微固相萃取的最佳工艺条件为:PCX用量25 mg,涡旋30 s,以3.0 mL 5%的氨-乙腈溶液进行洗脱。结论建立的含量测定方法可用于荷丹片中荷叶碱、O-去甲基荷叶碱、N-去甲基荷叶碱含量的分析测定。该方法简单精确,稳定性高;样品处理快捷简便,溶剂损耗明显减少;设备要求低,装置简便;分析速度快,分析周期短。
