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作 者:虞成华[1] 陆志芸[1] 葛宇[1] 忻元庆 宁啸骏[1] 印杰[1] 熊薇[1]
机构地区:[1]上海市质量监督检验技术研究院,上海200233 [2]上海市质量技术监督局,上海200233
出 处:《理化检验(化学分册)》2011年第3期261-265,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:上海市质量技术监督局立项资助项门(06TBT11;2009-23)
摘 要:提出了罐头食品中的双酚A、双酚A二缩水甘油醚及双酚A二缩水甘油醚的衍生物等7种化合物的液相色谱-串联质谱分析方法。样品经乙腈提取后,用正己烷净化,然后取下层清液蒸发至干。用乙腈-水(3+7)溶液溶解残渣,经Hypersil GOLD C_(18)色谱柱(2.1mm×100mm,3μm)分离,不同比例的乙酸铵溶液和甲醇的混合液为流动相作梯度淋洗,采用正离子模式多反应监测。7种化合物的质量浓度与其峰面积均在一定范围内呈线性关系,检出限(3S/N)均不大于2μg·L^(-1)。以罐头食品为基体,加入3种不同浓度的7种标准溶液做回收试验,测得平均回收率在80.0%~105.6%之间,相对标准偏差在3.2%~14%之间。LC-MS/MS was applied to the determination of bisphenol A (BPA), bisphenol A diglyeidyl ether (BAIZE) and its derivatives in canned food. Sample of canned food was extracted by aeetonitrile and purified by nhexane, and the clear lower phase obtained was evaporated to dryness. The residue was dissolved with acetonitrilewater (3+7) mixture and used for LC-MS/MS determination, in which Hypersil COLD C18 column (2. 1×100mm,3μm) was used as chromatographic column, and mixtures of ammonium acetate solution and methanol of different proportions were used as mobile phase in gradient elution; positive electrospray ionization as well as multiple reaction monitoring mode was used in the detection. Linear relationship between values of peak area and mass concentration of 7 compounds were obtained in definite ranges, with detection limit (3S/N) less than or equal to 2μg·L^- 1. Tests for recovery and precision were made by addition of standard solutions of the 7 standards in 3 different concentration levels to canned food sample which was then analyzed by the proposed method. Values of average recovery and RSD's (n=10) obtained were in the ranges of 80. 0%-105. 6% and 3. 2%-14% respectively.
关 键 词:液相色谱-串联质谱法 罐头食品 双酚A 双酚A二缩水甘油醚及其衍生物
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