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超高效液相色谱-质谱法测定环氧树脂粘结剂中双酚A

UHPLC-MS Determination of Bispheol A in Epoxy Resin Adhesives

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【作者】 赖莺董清木林睿葛秀秀蔡延平林海霞

【Author】 LAI Ying,DONG Qing-mu,LIN Rui,GE Xiu-xiu,CAI Yan-ping,LIN Hai-xia(Technical Center of Xiamen Entry-Exit Inspection and Quarantine Bureau,Xiamen 361026,China)

【机构】 厦门出入境检验检疫局技术中心

【摘要】 提出了环氧树脂粘结剂中双酚A的超高效液相色谱-质谱测定方法。样品用乙醇超声提取后,离心分离,取上清液过0.22μm有机滤膜,滤液经ZORBAX SB-C18色谱柱分离,用不同比例的水和乙腈的混合溶液作为流动相梯度淋洗,采用电喷雾负离子源,多反应监测模式。双酚A的质量浓度在2~1 000μg.L-1范围内与其峰面积呈线性关系,测定下限(10S/N)为0.5mg.kg-1。以空白环氧树脂粘结剂为基体,进行加标回收试验,测得回收率在89.3%~93.2%之间,测定值的相对标准偏差(n=6)在1.8%~3.3%之间。

【Abstract】 UHPLC-MS was applied to the determination of bisphenol A in epoxy resin adhesives.Sample of epoxy resin adhesives was extracted by ethanol,after centrifugation,the clear super natant obtained was filtrated with 0.22 μm organic filtration membrane.The filtrate was used for UHPLC-MS determination,in which ZORBAX SB-C18 column was used as chromatographic column,and mixtures of water and acetonitrile of different proportions were used as mobile phase in gradient elution;negative electrospray ionization as well as multiple reaction monitoring mode was used in the detection.Linear relationship between value of peak area and mass concentration of bisphenol A was obtained in the range of 2-1 000 μg·L-1,with quantification limit(10S/N) of 0.5 mg·kg-1.Tests for recovery and precision were made by addition of standard solution of bispheol A to blank sample of epoxy resin adhesives which was then analyzed by the proposed method.Values of recovery and RSD′s(n=6) obtained were in the ranges of 89.3%-93.2% and 1.8%-3.3% respectively.

【基金】 国家质检总局课题(2011IK048;2009IK075)
  • 【文献出处】 理化检验(化学分册) ,Physical Testing and Chemical Analysis(Part B:Chemical Analysis) , 编辑部邮箱 ,2013年04期
  • 【分类号】O657.63;TQ433.437
  • 【被引频次】2
  • 【下载频次】166
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