高效液相色谱法测定牛奶和奶粉中的脱氢乙酸

Determination of dehydroacetic acid in milk and milk powder by high performance liquid chromatography

中文关键词:  高效液相色谱法  牛奶和奶粉  脱氢乙酸

英文关键词:high performance liquid chromatography  milk and milk powder  dehydroacetic acid

中文摘要:

      目的 建立测定牛奶和奶粉中的脱氢乙酸的高效液相色谱法(high performance liquid chromatography, HPLC)。方法 样品用硫酸铜溶液和氢氧化钠溶液沉淀蛋白, 其中的脱氢乙酸用10%的乙醇溶液进行提取, 以甲醇+0.02 mol/L的乙酸铵溶液(用氨水调pH=8.0)作为流动相进行梯度洗脱, 经TechMate C18色谱柱 (4.6 mm×250 mm, 5 μm)分离, 在波长292 nm处进行检测。结果 此方法的线性范围是1.003~100.336 μg/mL, 相关系数r=0.9999, 以3倍信噪比计算检出限为0.1 μg/mL。加标回收率为87.2%~95.3%, 相对标准偏差(relative standard deviation, RSD)为1.5%~3.9%。结论 此方法简便快速, 准确可靠, 灵敏度高, 可用于牛奶和奶粉中脱氢乙酸的检测。

英文摘要:

      Objective To establish a method for determination of dehydroacetic acid in milk and milk powder by high performance liquid chromatography (HPLC). Method The samples were precipitated with copper sulfate solution and sodium hydroxide solution. The dehydroacetic acid was extracted with 10% ethanol solution, and the gradient elution was performed with methanol+0.02 mol/L ammonium acetate solution (pH=8.0 with ammonia). Then they were separated by Tech-Mate C18 column (4.6 mm×250 mm, 5 μm) and detected at the wavelength of 292 nm. Results The linear range of this method was 1.003-100.336 μg/mL with the correlation coefficient (r) of 0.9999. The limit of detection was 0.1 g/mL (S/N=3). The recovery rates were 87.2%-95.3%, and relative standard deviations (RSD) were 1.5%-3.9%. Conclusion This method is simple, rapid, accurate, reliable and sensitive, which is suitable for the detection of dehydrogenacetic acid in milk and milk powder.