高效液相色谱法检测葡萄糖酸-δ-内酯
Determination of gluconic acid-δ-lactone by high performance liquid chromatography
师保炜 1吴艳阳 1武斌 1纪利俊 1陈葵1
作者信息
- 1. 华东理工大学 化工学院,上海 200237
- 折叠
摘要
葡萄糖酸-δ-内酯常通过葡萄糖酸水溶液蒸发浓缩制备,所得产品常含有少量的葡萄糖酸和葡萄糖酸-γ-内酯.为了检测产品中葡萄糖酸-δ-内酯的质量分数,文中建立了可快速分离分析葡萄糖酸-δ-内酯、葡萄糖酸和葡萄糖酸-γ-内酯的高效液相色谱法,并优化了葡萄糖酸-δ-内酯的分析条件.以SPD-M20A二极管阵列检测器,采用Titank Hilic色谱柱分离葡萄糖酸-δ-内酯、葡萄糖酸和葡萄糖酸-γ-内酯,以0.01 mol/L乙腈-磷酸水溶液(体积比90∶10)为流动相进行等度洗脱,柱温为30℃,流速为1.0 mL/min,检测波长为205 nm,进样量为20 μL.结果表明,葡萄糖酸-δ-内酯在7 min内可实现较好的分离;在0.5-2.5 mg/mL内具有良好的线性关系(r＞0.999),检出限为0.002 mg/mL,定量限为0.5 mg/mL,3个水平的平均加标回收率为98.8％-99.9％,相对标准偏差0.1％-0.4％(n=5).此方法分析时间短、灵敏度高、分离效果好,可用于葡萄糖酸-δ-内酯、葡萄糖酸和葡萄糖酸-γ-内酯的同时检测.
Abstract
Gluconic acid-δ-lactone is often prepared by evaporation concentration from gluconic acid aqueous solution and contains a small amount of gluconic acid and gluconic acid-γ-lactone.In order to determine gluconic acid-δ-lactone in the product,a high-performance liquid chromatography method for the rapid separation and anylysis of gluconic acid-δ-lactone,gluconic acid and gluconic acid-γ-lactone was established and the conditions were optimized for the determination of gluconic acid-δ-lactone.The Titank Hilic column was chosen for the separation of gluconic acid-δ-lactone,gluconic acid and gluconic acid-γ-lactone.The mobile phase was 0.01 mol/L acetonitrile-phosphoric acid aqueous solution(volume ratio 90:10),the column temperature was 30° C,the flow rate was 1.0 mL/min,the detection wavelength was 205 nm,and the injection volume was 20 μL.The results show that gluconic acid-δ-lac tone can be well detected within 7 min.Gluconic acid-δ-lactone presentes a good linear relationship(r＞0.999)in the mass concentration range of 0.5-2.5 mg/mL,the detection limit is 0.002 mg/mL,the limit of quantification is 0.5 mg/mL,the average spiked recovery of the three levels is 98.8％-99.9％,and the relative standard deviation is 0.1％-0.4％(n=5).This method characterizes short analysis time,high sensitivity and good separation effect,and can be used to determine gluconic acid-δ-lactone,gluconic acid and gluconic acid-γ-lactone simultaneously.
关键词
高效液相色谱/二极管阵列检测器/Hilic色谱柱/葡萄糖酸-δ-内酯/葡萄糖酸/葡萄糖酸-γ-内酯Key words
high performance liquid chromatography/diode array detectors/Hilic chromatography column/gluconic acid-δ-lactone/gluconic acid/gluconic acid-γ-lactone引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
万方数据