食品研究与开发
食品研究與開髮
식품연구여개발
FOOD RESEARCH AND CEVELOPMENT
2013年
17期
80-82,83
,共4页
刘艳琴%王浩%杨红梅%郭启雷%史海良%田艳玲
劉豔琴%王浩%楊紅梅%郭啟雷%史海良%田豔玲
류염금%왕호%양홍매%곽계뢰%사해량%전염령
液质联用仪%婴儿配方乳粉%双酚A%己烯雌酚
液質聯用儀%嬰兒配方乳粉%雙酚A%己烯雌酚
액질련용의%영인배방유분%쌍분A%기희자분
LC-MS-MS%infant milk powder%Biphenol A%diethylstilbestrol
建立了婴儿乳粉中双酚A和己烯雌酚残留的高效液相色谱-串联四极杆质谱联用测定方法。样品经碱性乙腈超声提取，以MGⅢ-C18色谱柱（2.1×150 mm，1.8μm）分离，流动相为10 mmol/L乙酸铵水溶液和甲醇（梯度洗脱），流速0.25 mL/min。采用多反应监测负离子模式，可以同时对婴幼儿配方乳粉中的双酚A和己烯雌酚进行定性和定量测定。方法在1.0μg/L～25.0μg/L范围内呈良好线性，方法的检出限为5μg/kg。在5、25、250μg/kg三个加标水平下，加标回收率为80.6%～102.9%，相对标准偏差为1.29%～8.83%。
建立瞭嬰兒乳粉中雙酚A和己烯雌酚殘留的高效液相色譜-串聯四極桿質譜聯用測定方法。樣品經堿性乙腈超聲提取，以MGⅢ-C18色譜柱（2.1×150 mm，1.8μm）分離，流動相為10 mmol/L乙痠銨水溶液和甲醇（梯度洗脫），流速0.25 mL/min。採用多反應鑑測負離子模式，可以同時對嬰幼兒配方乳粉中的雙酚A和己烯雌酚進行定性和定量測定。方法在1.0μg/L～25.0μg/L範圍內呈良好線性，方法的檢齣限為5μg/kg。在5、25、250μg/kg三箇加標水平下，加標迴收率為80.6%～102.9%，相對標準偏差為1.29%～8.83%。
건립료영인유분중쌍분A화기희자분잔류적고효액상색보-천련사겁간질보련용측정방법。양품경감성을정초성제취，이MGⅢ-C18색보주（2.1×150 mm，1.8μm）분리，류동상위10 mmol/L을산안수용액화갑순（제도세탈），류속0.25 mL/min。채용다반응감측부리자모식，가이동시대영유인배방유분중적쌍분A화기희자분진행정성화정량측정。방법재1.0μg/L～25.0μg/L범위내정량호선성，방법적검출한위5μg/kg。재5、25、250μg/kg삼개가표수평하，가표회수솔위80.6%～102.9%，상대표준편차위1.29%～8.83%。
A quick confirmative method was developed for determining the residues of Bisphenol A and diethylstilbestrol in infant milk powder by LC-MS/MS. The sample was ultrasonic extracted with alkaline acetonitrile, the HPLC separation was carried out on a MGⅢ-C18 column (2.1×150 mm, 1.8μm) ,the mobile phase were 10 mmol/L ammonium acetate solution and methanol with gradient elution, the flow was 0.25 mL/min. The detection of Bisphenol A and diethylstilbestrol was carried outin the negative multi-reaction monitoring (MRM)mode. Under the optimal conditions, good linear relationship was obtained in the range of 1.0 μg/L-25.0 μg/L for Bisphenol A and diethylstilbestrol.The limit of detection was 5μg/kg. The recoveries at three spiked levels of 5,25,250 μg/kg were between 80.6%and 102.9%, and RSDs value were between 1.29%and 8.83%.
