通过碱性溶液提取,再用正己烷萃取除去脂肪,用乙酸调p H为酸性条件后用乙酸乙酯-异丙醇反萃取,浓缩后再通过混合阴离子固相萃取柱净化,最后采用高效液相色谱分离检测。结果:三种复合硝基酚钠组分在0.051.0μg/m L范围内其浓度与峰面积呈线性,相关系数均可达到0.999;通过萃取、反萃取以及固相萃取等多种手段净化,样品基质几乎无干扰,检出限可达到0.0030.005 mg/kg;通过对0.25、0.5、1.0μg进行加标测试,其回收率在81%95%之间,相对标准偏差均小于10%。
This method gave an account that extracted by alkaline solution,extracted by hexane to remove the fat,back-extraction with ethyl acetate-isopropanol under acid condition,purified by mixing anionic solid-phase extraction(SPE),finally,using liquid chromatography(HPLC) for testing.The three kinds of compound sodium nitrophenol components concentration and the peak area was linear correlation within the scope of 0. 05 ~1.0 μg/m L. The correlation was 0.999. Through the extraction,back extraction and a variety of means such as solid phase extraction purification,the sample almost had no interference,so the detection limit could reached0.003~0.005 mg/kg. Through the standard addition test of 0.25,0.5,1.0 μg,its recovery was between 81%~95%,relative standard deviation was less than 10%.