蔗糖-6-乙酯是制备三氯蔗糖的关键中间体,建立一种准确、快速的分析方法测定蔗糖-6-乙酯是这种甜味剂生产质控关键。采用高效液相色谱-蒸发光散射法(high performance liquid chromatography-evaporative light scattering detector,HPLC-ELSD)检测蔗糖-6-乙酯,使用ZORBAX SB-Aq色谱柱,以甲醇水溶液(V(甲醇)∶V(水)=5∶90)为流动相,流速为0.8 mL/min,蒸发光漂移管温度为85 ℃,氮气流速为1.5 L/min。同时对内标法及外标法检测蔗糖-6-乙酯进行了方法学验证。实验表明,2种方法的线性范围均为1.10~11.03 g/L,线性相关系数均在0.99以上,其中外标法的RSD值均小于3.0%,而内标法的RSD值均小于2.0%,并且内标法的检出限和定量限均低于外标法,分别为31.04及103.46 μg/mL。2种方法均能检测蔗糖-6-乙酯,其中内标法略优于外标法。该研究建立的方法可用于蔗糖-6-乙酯的含量检测,并为蔗糖酯的检测分析提供了参考。
Sucrose-6-acetate is a key intermediate for sucralose preparation. Establishing an accurate and rapid analytical method for the determination of sucrose-6-acetate is essential for the quality control in sucralose production. Sucrose-6-acetate was detected by high performance liquid chromatography-evaporative light scattering (HPLC-ELSD). The analytical column was ZORBAX SB-Aq column with methanol/water (5∶90, V/V) as the mobile phase at a flow rate of 0.8 mL/min. The evaporative light drift tube temperature was 85 ℃ and the nitrogen flow rate was 1.5 L/min. The method was verified by internal standard method and external standard method for the detection of sucrose-6-acetate. The linear range of both methods was 1.10-11.03 mg/mL, with the linear correlation coefficient of above 0.99. The RSD value of the external standard method was less than 3.0%, and that of the internal standard method was less than 2.0%. In addition, the detection limit and quantification limit of the internal standard method were lower than the external standard method, which were 31.04 mg/mL and 103.46 mg/mL, respectively. Both methods could detect sucrose-6-acetate, and the internal standard method was slightly better than the external standard method. The method established in this study can be used for the determination of sucrose-6-acetate, which provides a reference for the detection and analysis of sucrose esters.
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