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

作　　者：师保炜 吴艳阳[1] 武斌[1] 纪利俊[1] 陈葵[1] SHI Baowei;WU Yanyang;WU Bin;JI Lijun;CHEN Kui(School of Chemical Engineering,East China University of Science&Technology,Shanghai 200237,China)

机构地区：[1]华东理工大学化工学院,上海200237

出　　处：《化学工程》2024年第6期1-5,32,共6页Chemical Engineering(China)

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20μL。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。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 9010),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 20μL.The results show that gluconic acid-δ-lactone 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 

分 类 号：O657.72[理学—分析化学]