CAJ | 학술논문

本文建立了鲜牛乳及奶粉中4种雌激素（17β-雌二醇、雌三醇、雌酮、己烯雌酚）的HPLC分析方法。奶粉样品溶解于水，QuEChERS方法萃取，用乙腈沉淀蛋白质并提取雌激素，正己烷除脂，经氨基柱净化，C18色谱柱分离，采用紫外检测器，检测波长为230 nm。该方法对鲜牛乳及奶粉中17β-雌二醇、雌三醇、雌酮、己烯雌酚的检出限（S/N=3计）分别为0.03 mg/kg、0.026 mg/kg、0.03 mg/kg、0.012 mg/kg和0.024 mg/kg、0.021 mg/kg、0.025 mg/kg、0.01 mg/kg。定量限（以S/N=10计）分别为0.1 mg/kg、0.09 mg/kg、0.1 mg/kg、0.04 mg/kg和0.07 mg/kg、0.07 mg/kg、0.08 mg/kg、0.03 mg/kg在0.1、1.0、2.0 mg/kg 三个浓度水平添加的平均回收率在81%~97%的范围内，RSD值在3.2%~8.7%之间。
본문건립료선우유급내분중4충자격소（17β-자이순、자삼순、자동、기희자분）적HPLC분석방법。내분양품용해우수，QuEChERS방법췌취，용을정침정단백질병제취자격소，정기완제지，경안기주정화，C18색보주분리，채용자외검측기，검측파장위230 nm。해방법대선우유급내분중17β-자이순、자삼순、자동、기희자분적검출한（S/N=3계）분별위0.03 mg/kg、0.026 mg/kg、0.03 mg/kg、0.012 mg/kg화0.024 mg/kg、0.021 mg/kg、0.025 mg/kg、0.01 mg/kg。정량한（이S/N=10계）분별위0.1 mg/kg、0.09 mg/kg、0.1 mg/kg、0.04 mg/kg화0.07 mg/kg、0.07 mg/kg、0.08 mg/kg、0.03 mg/kg재0.1、1.0、2.0 mg/kg 삼개농도수평첨가적평균회수솔재81%~97%적범위내，RSD치재3.2%~8.7%지간。
A novel method for the determination of 4 estrogens(17β-estradiol,Estriol,Estrone and Diethylstilbestrol)in raw milk and milk powder has been developed by HPLC. The milk powder was dissolved in water and then it was extracted with acetonitrile by QuEChERS method and purified by NH2 solid phase extraction cartridge after fats were removed by hexane. The analyte was separated on a C18 column (Waters Atlantis dC18, 4.6 × 250 mm , i.d 5μm) at UV 230 nm. The detection limits(S/N=3) of 17β-estradiol, estriol, estrone and diethylstilbestrol in milk powder and fresh milk were 0.03 mg/kg, 0.026 mg/kg, 0.03 mg/kg, 0.012 mg/kg and 0.024 mg/kg, 0.021 mg/kg, 0.025 mg/kg, 0.01 mg/kg, respectively. The quantitation limit(S/N=10) in milk powder and raw milk were 0.1 mg/kg, 0.09 mg/kg, 0.1 mg/kg, 0.04 mg/kg and 0.07 mg/kg, 0.07 mg/kg, 0.08 mg/kg, 0.03 mg/kg, respectively. The recoveries were 81%~97%with the range of RSD from 3.2%to 8.7%.