A method was established of reversed-phase high performance liquid chromatography for the determination of sucrose-6-acetate.In the method,SupelcosilTMLC-18（250mm×4.6mm i.d.5μm）was used as chromatographic colu...A method was established of reversed-phase high performance liquid chromatography for the determination of sucrose-6-acetate.In the method,SupelcosilTMLC-18（250mm×4.6mm i.d.5μm）was used as chromatographic column and V（acetonitrile）∶V（methanol）∶V（water）=10∶10∶80 as mobile phase.The linear ranges was 0.5mg/L～900mg/L.The lower limit of detection of surose-6-acetate was 0.2mg/L.The recovery of the method was 98.53% and the relative standard deviations was 0.95%.By the method,the reaction raw materials,the reaction mediates and the reaction products could be separated effcctively,and the reaction progress could also be indicated directly.展开更多
The separation and purification of sucrose6-acetate from acetylation product of sucrose by PUROLITE PCR(Ca) ion exchange resin were invesigaged.It was found that the adsorption velocity of sucrose-6-acetate on ion exc...The separation and purification of sucrose6-acetate from acetylation product of sucrose by PUROLITE PCR(Ca) ion exchange resin were invesigaged.It was found that the adsorption velocity of sucrose-6-acetate on ion exchange resin was corresponding to sucrose,but the dynamic permeable adsorption capacity of sucrose was larger than that of sucrose-6-caetate.The resolution of the samples on column chromatography could generally be enhanced with the increase of the ration of column height to diameter,decreased with the increase of the loading quantity and the flowing velocity.Under the typical separation operation conditions,the content of sucrose-6-acetate could reach about 94 from 80.7%,and the average separation yield was about 85.0%.展开更多
以蔗糖-6-乙酯为原料,Vilsmeier试剂为氯化剂,对蔗糖-6-乙酯进行选择性氯化,制得三氯蔗糖-6-乙酯,在碱性条件下脱除乙酰基,制得三氯蔗糖。考察了反应温度、反应时间对氯化反应的影响,碱的种类、反应温度和pH值对脱乙酰基反应的影响。研...以蔗糖-6-乙酯为原料,Vilsmeier试剂为氯化剂,对蔗糖-6-乙酯进行选择性氯化,制得三氯蔗糖-6-乙酯,在碱性条件下脱除乙酰基,制得三氯蔗糖。考察了反应温度、反应时间对氯化反应的影响,碱的种类、反应温度和pH值对脱乙酰基反应的影响。研究结果表明:在110℃条件下,蔗糖-6-乙酯与Vilsmeier试剂反应2h,三氯蔗糖-6-乙酯收率较好,为51.9%;在-10℃条件下,用KOH溶液调节pH=9,反应4h得到三氯蔗糖,收率为80.2%。产物结构经IR、1 H NMR、13 CNMR表征分析。展开更多
文摘A method was established of reversed-phase high performance liquid chromatography for the determination of sucrose-6-acetate.In the method,SupelcosilTMLC-18（250mm×4.6mm i.d.5μm）was used as chromatographic column and V（acetonitrile）∶V（methanol）∶V（water）=10∶10∶80 as mobile phase.The linear ranges was 0.5mg/L～900mg/L.The lower limit of detection of surose-6-acetate was 0.2mg/L.The recovery of the method was 98.53% and the relative standard deviations was 0.95%.By the method,the reaction raw materials,the reaction mediates and the reaction products could be separated effcctively,and the reaction progress could also be indicated directly.
文摘The separation and purification of sucrose6-acetate from acetylation product of sucrose by PUROLITE PCR(Ca) ion exchange resin were invesigaged.It was found that the adsorption velocity of sucrose-6-acetate on ion exchange resin was corresponding to sucrose,but the dynamic permeable adsorption capacity of sucrose was larger than that of sucrose-6-caetate.The resolution of the samples on column chromatography could generally be enhanced with the increase of the ration of column height to diameter,decreased with the increase of the loading quantity and the flowing velocity.Under the typical separation operation conditions,the content of sucrose-6-acetate could reach about 94 from 80.7%,and the average separation yield was about 85.0%.
文摘以蔗糖-6-乙酯为原料,Vilsmeier试剂为氯化剂,对蔗糖-6-乙酯进行选择性氯化,制得三氯蔗糖-6-乙酯,在碱性条件下脱除乙酰基,制得三氯蔗糖。考察了反应温度、反应时间对氯化反应的影响,碱的种类、反应温度和pH值对脱乙酰基反应的影响。研究结果表明:在110℃条件下,蔗糖-6-乙酯与Vilsmeier试剂反应2h,三氯蔗糖-6-乙酯收率较好,为51.9%;在-10℃条件下,用KOH溶液调节pH=9,反应4h得到三氯蔗糖,收率为80.2%。产物结构经IR、1 H NMR、13 CNMR表征分析。
