柱前衍生高效液相色谱法测定奶粉中糠醛类化合物

Determination of furfural compounds in infant formula by precolumn derivatization and high performance liquid chromatography

建立了高效液相色谱法(HPLC)测定婴幼儿配方奶粉中4种糠醛类化合物含量的分析方法,研究不同保存环境温度对奶粉中4种糠醛类化合物含量的影响。前处理采用柱前衍生,同时考察方法的线性关系、精密度、加标回收率、检出限以及定量限等指标,采用外标法定量。结果表明:该方法在0~20μg范围内线性良好(R^(2)> 0.999),4种糠醛类化合物(羟甲基糠醛、糠醛、2-呋喃甲基酮和甲基糠醛)检出限分别为50,20,30,30μg/kg,定量限分别为150,60,90,90μg/kg,平均加标回收率在83.3%~97.6%范围内,相对标准偏差均小于10%。当奶粉保存环境温度高于30℃,随着温度升高,4种糠醛类化合物含量呈上升趋势,尤以羟甲基糠醛与糠醛增幅明显。该研究方法能满足婴幼儿配方奶粉中糠醛类化合物的测定,同时为奶粉保质期量化提供参考。

A high performance liquid chromatography( HPLC) method for the determination of four furfural compounds in infant formula was established. The effect of different storage temperatures on the contents of four furfural compounds in infant formula were studied. Precolumn derivatization was used in the pretreatment,and the linear relationship,precision,recovery rate,detection limit and quantification limit of the method were investigated. The linear range of the method was 0-20 μg( R^(2)> 0. 999). The detection limits of four furfural compounds( hydroxymethyl furfural,furfural,2-furyl methyl ketone and methyl furfural) were 50,20,30,30 μg/kg,and the limits of quantification were 150,60,90,90 μg/kg,respectively,The average recoveries ranged from 83. 3% to 97. 6%,and the relative standard deviations were less than 10%. When the storage temperature of milk powder was higher than 30℃,the contents of four furfural compounds increased with the increase of temperature,especially hydroxymethyl furfural and furfural. The method can be used for the determination of furfural compounds in infant formula.