高效液相色谱-串联质谱法测定婴幼儿乳粉中甲醛残留

Determination of formaldehyde residues in infant formula milk powder by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  婴幼儿配方乳粉  甲醛  2,4-二硝基苯肼  高效液相色谱-串联质谱法

英文关键词:infant formula milk powder  formaldehyde  2,4-dinitrobenzenehydrazine  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立一种高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定婴幼儿乳粉中甲醛残留量的分析方法。方法 婴幼儿乳粉中的甲醛通过2,4-二硝基苯肼-乙酸钠缓冲溶液衍生得到甲醛-2,4-二硝基苯腙化合物, 经过色谱柱BEH C18 (2.1 mm×50 mm, 1.7 μm)分离, 以0.1%甲酸水溶液:乙腈=3:7(V:V)为流动相进行等度洗脱, 柱温40 ℃, 流速0.4 mL/min, 多反应模式监测, 外标法定量。结果 甲醛衍生物在0.1~1000 μg/L内线性关系良好且相关系数(r2)大于0.99。方法检出限和定量限分别为0.3 μg/kg 和1.0 μg/kg, 在2.5、5.0、10 mg/kg水平添加下婴幼儿乳粉中甲醛衍生物的平均加标回收率为87.9%~92.7%, 相对标准偏差小于2.7%(n=6)。结论 该方法具有快速简便、准确度好、灵敏度高等特点, 适用于婴幼儿乳粉体系中甲醛的测定。

英文摘要:

      Objective To establish a method for determination of formaldehyde in infant formula milk powder by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods Formaldehyde in infant formula milk powder was derived from 2,4-dinitrobenzenehydrazine-sodium acetate buffer solution to formaldehyde-2,4-dinitrobenzenehydrazone, which was separated by BEH C18 chromatographic column (2.1 mm× 50 mm, 1.7 μm) and analyzed by HPLC-MS/MS with 0.1% formic acid solution-acetonitrile (3:7, V:V) as the mobile phase, the column temperature was 40 ℃, the flow rate was 0.4 mL/min. It was monitored by multi reaction mode, and quantified by external standard method. Results Formaldehyde derivative had good linear relationships in the concentration of 0.1-1000 μg/L (r2>0.99). The limit of detection and limit of quantitation were 0.1 μg/kg and 1 μg/kg, respectively. The average recoveries were 87.9%-92.7% at the spiked levels of 2.5, 5, 10 mg/kg and the relative standard deviations were less than 2.7% (n=6). Conclusion The method is rapid and simple, accurate and sensitive, which is suitable for determination of formaldehyde in infant formula milk powder.