【作者】 邱文龙；

【导师】 王仲孚；

【作者基本信息】 西北大学 ， 细胞生物学， 2008， 硕士

【摘要】 三氯蔗糖,化学名4,1’,6’-三氯-4,1’,6’-三脱氧半乳蔗糖,是目前世界上高甜度非营养型甜味剂开发研究最高水平的产物。具有甜度高、不参与代谢、热量值为零、性质稳定、风味纯正等优点,已广泛用于食品及医药添加剂。本研究采用全基团保护法合成了三氯蔗糖,建立了完整的三氯蔗糖及其中间体的分析检测方法,可望为规模化生产提供在线监测手段。（1）中间体6,1’,6’-三氧三苯甲基-五乙酰基蔗糖（TRISPA）采用RP-HPLC分析检测。Waters XTerraTM RP₁₈5μm,3.9×150 mm色谱柱;以乙腈:水（84∶16）作流动相;流速0.6 mL/min;检测波长为234 nm;TRISPA在0.05-0.8 mg/mL范围内线性良好,检测限为5 ng（S/N=3）;相对标准偏差为0.34%,平均回收率为99.2%。（2）中间体2,3,4,3’,4’-五乙酰基蔗糖（4-PAS）和2,3,6,3’,4’-五乙酰基蔗糖（6-PAS）经过硅醚化衍生后,采用气质联用定性,气相色谱定量,肌醇六乙酸酯为内标。4-PAS的硅醚衍生物在0.05-0.8 mg/mL范围内线性良好,检测限为0.2 ng（S/N=3）,相对标准偏差（RSD）为0.562%,平均回收率为98.1%。6-PAS的硅醚衍生物与4-PAS得到了基线分离。4-PAS向6-PAS的转化实现了实时监控。（3）中间体4,1’,6’-三氯-4,1’,6’-三脱氧半乳蔗糖五乙酸酯（TOSPA）采用高效液相色谱紫外检测器法分析检测。色谱柱:Waters XTerraTM RP₁₈5μm,3.9×150 mm;以乙腈:水（50:50）作流动相;流速0.6 mL/min;检测波长为229 nm;TOSPA的质量在0.0125-0.1000 mg范围内线性良好,方法的检测限为10 ng（S/N=3）。相对标准偏差（RSD）为1.15%,平均回收率为97.24%。（4）三氯蔗糖经过硅醚化衍生后采用气质联用定性,气相色谱定量,肌醇六乙酸酯为内标。三氯蔗糖衍生物在0.005-0.06mg/mL浓度范围内线性良好,检测限为0.25 ng（S/N=3）,相对标准偏差（RSD）为0.626%,平均回收率为97.95%。更多还原

【Abstract】 Sucralose（1,6-dichloro-1,6-dideoxy-beta-D-fructofuranosyl-4-chloro-4-deoxy-alpha -D-galactopyranoside）is a high-intensity sweetener derived from sucrose and it is regarded as the highest accomplishment of intense sweetener.Due to its high sweetness,obvious sweetener characteristics and safety,sucralose is used in the manufacturing of artificially sweetened food and drug products.In this paper, sucralose was synthesized using path-of-hologroup-protected as well as methods for the analysis of sucralose and its intermediates were developed.6,1’,6’-Tri-O-tritylsucrose-penta-acetate（TRISPA）was analysed by RP-HPLC. The column was Waters XTerra^TMRP₁₈5μm,3.9×150mm;The mobile phase was acetonitrile:water（84:16）;The flow rate was 0.6 mL/min;TRISPA was determined with UV detector at 234 nm.Good linearities were obtained within the range from 0.05 to 0.8 mg/mL and the minimum limit of detection was 5 ng（S/N=3）.The average recovery of samples were 99.2%and the relative standard derivation was 0.34%.（2）4-PAS and 6-PAS were converted into their trimethylsilyl（TMS）ethers,then identified and quantified by GC-MS and GC respectively,using myo-inositol ester as the internal standard.Good linearities of their TMS ethers were obtained within the range from 0.05 to 0.8 mg/mL of the 4-PAS TMS ether and the minimum limit of detection was 0.25 ng（S/N=3）.Precision expressed by the relative standard deviation （RSD）was 0.526%.The average recovery of the method was 98.1%.The 6-PAS TMS ether has a good separation from 4-PAS TMS ether and the conversion process of 4-PAS to 6-PAS was monitored.（3）TOSPA was analysed using RP-HPLC.The column was Waters XTerra^TM RP₁₈5μm,3.9×150 mm;The mobile phase was acetonitrile:water（50:50）;The flow rate was 0.6 mL/min;TOSPA was determined with UV detector at 229 nm.Promising linearities were obtained within the range from 0.0125 to 0.1000 mg and the minimum limit of detection was 10 ng（S/N=3）.The average recovery of samples were 97.2% and the relative standard derivation was 1.15%.（4）Sucralose was converted into its trimethylsilyl（TMS）ether,then qualified and quantified by GC-MS,GC respectively,using myo-inositol ester as the internal standard.Good linearities of its TMS ethers were obtained within the range from 0.005 to 0.06 mg/mL of the Sucralose TMS ether and the minimum of detection was 0.25 ng（S/N=3）.Precision in terms of RSD was 0.626%and the average recovery was 97.95%.更多还原