HPLC-示差折光检测法测定白酒中三氯蔗糖的方法研究

Determination of sucralose in Baijiu by high performance liquid chromatography-refractive index detector

该研究采用高效液相色谱-示差折光检测法测定白酒中的三氯蔗糖含量,从流动相比例、流速、进样量、柱温、示差检测池温度五个方面进行考察,确定最佳色谱条件。结果表明,在流动相为乙腈∶水(20∶80,V/V)、流速1.0 mL/min、进样量20μL、柱温35℃、示差折光检测器温度35℃条件下,三氯蔗糖在质量浓度0.01~0.40 mg/mL范围内,线性关系好,相关系数R2=0.99994,检出限为3.538μg/mL,定量限为11.79μg/mL,平均加标回收率为96.3%~103.4%,精密度试验结果相对标准偏差在0.6%~6.6%之间,均能满足检测要求。该方法操作简单、方便快捷、定量准确,适用于白酒中三氯蔗糖含量的大规模、大批量快速检测分析。

In this study,the content of sucralose in Baijiu(Chinese liquor)was determined by high performance liquid chromatography-refractive index detector(HPLC-RID),and the optimal chromatographic conditions were determined from five aspects:mobile phase ratio,flow rate,injection volume,column temperature and RID cell temperature.The results showed that under the conditions of acetonitrile∶water(20∶80,V/V)as mobile phase,flow rate 1.0 ml/min,injection volume 20μl,column temperature 35℃,differential refraction detector(RID)temperature 35℃,sucralose showed a good linear relationship within the range of 0.01-0.40 mg/ml,the correlation coefficient R2=0.99994,the detection limit was 3.538μg/ml,the quantitative limit was 11.79μg/ml,the average recovery rate of the standard was 96.3%-103.4%,and the relative standard deviation of the precision tests results was between 0.6%-6.6%,all could met the detection requirements.The method was simple,convenient and accurate,and was suitable for the large-scale rapid detection and analysis of sucralose content in Baijiu.