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作 者:李少霞[1] 黄伟雄[1] 余胜兵[1] 刘锐[1] 陈明[1] 姚敬[1]
出 处:《理化检验(化学分册)》2013年第6期679-682,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:广东省医学科研基金(A2011062)
摘 要:提出了气相色谱-质谱法测定奶瓶中双酚A含量的方法。取剪碎的样品经二氯甲烷溶解,甲醇提取后,所得净化液中双酚A与N,O-双(三甲基硅烷基)三氟乙酰胺-三甲基氯硅烷(99+1)溶液进行衍生化反应,产物用乙酸乙酯定容。在气相色谱分离中用DB-5MS毛细管柱为固定相,在质谱分析中采用选择离子监测模式。双酚A的质量浓度在10.0~200.0μg·L-1范围内与峰面积呈线性关系,测定下限(10S/N)为1.0mg·kg-1。方法用于奶瓶中双酚A的测定,回收率在77.5%~95.1%之间,相对标准偏差(n=6)为3.9%。A method of GC-MS for determination of bisphenol A in feeding-bottle was proposed.The sheared sample was dissolved with CH2Cl2 and extracted with methanol,then derivatized with N,O-bis(trimethyl-silanyl)-trifluoro-acetamide-trimethylchloro silane(99+1) solution.The derivatized product was dissolved with ethyl acetate.DB-5MS capillary column was used for GC separation and selected ion monitoring mode were adopted in MS determination.Linear relationship between values of peak area and mass concentration of bisphenol A was obtained in the range of 10.0-200.0 μg·L-1,with lower limit of determination(10S/N) of 1.0 mg·kg-1.The proposed method was applied to the analysis of feeding-bottle,giving values of recovery in the range of 77.5%-95.1% and RSD(n=6) of 3.9%.
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