乳制品中邻苯二甲酸酯类化合物残留量检测方法

建立了测定乳制品中邻苯二甲酸之类物质残留量的气质联用方法。液体乳及含乳饮料采用正己烷萃取后直接测定;乳粉类样品先用正己烷萃取、再用凝胶萃取小柱净化后上机测定。色谱测定条件为采用DB-5MS(30 m×0.25 mm×0.25μm)石英毛细管柱梯度升温进行分离质谱条件为色谱与质谱接口温度280℃、电子轰击源、选择离子扫描模式、电力能量70 eV。通过各组分的定性与定量离子分别对邻苯二甲酸酯进行定性、定量测定。该方法样品加标回收率分别在86%~105%之间,液体乳及乳饮料检出限为0.05 mg/kg,乳粉为0.1 mg/kg。本法具有操作简单、测定快速、灵敏度高、专属性及准确性好等优点。

Phthalates in milk residue detection method

Established for the determination of phthalate esters dairy residues of substances by GC method.Milk and milk beverages measured directly after extraction using n-hexane;milk samples of the first class with n-hexane extraction,gel extraction column and then purified on the machine.Chromatographic conditions for the use of DB-5ms(30 m × 0.25 mm × 0.25 μm) capillary column for separation temperature gradient chromatography and mass spectrometry mass spectrometry conditions for the interface temperature of 280 ℃,electron impact source,selected ion scan mode,the power energy 70 eV.Through the qualitative and quantitative components of the phthalate ion,respectively,qualitative and quantitative determination.The method of standard addition sample recoveries were between 86%~105%,Milk and milk drinks detection limit of 0.05 mg/kg,milk powder is 0.1 mg/kg.This method is simple,rapid determination,high sensitivity,specificity and accuracy good.