UHPLC-MS Determination of Bispheol A in Epoxy Resin Adhesives
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0.22 μm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2~1 000 μg·L-1范围内与其峰面积呈线性关系,测定下限(10S/N)为0.5 mg·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.
中图分类号 O657.63
所属栏目 工作简报
基金项目 国家质检总局课题(2011IK048;2009IK075)
收稿日期 2012/1/2
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备注赖莺(1978-),女,福建长汀人,高级工程师,博士,主要从事色谱、质谱和光谱等方面的进出口商品检验和科研工作。
引用该论文: LAI Ying,DONG Qing-mu,LIN Rui,GE Xiu-xiu,CAI Yan-ping,LIN Hai-xia. UHPLC-MS Determination of Bispheol A in Epoxy Resin Adhesives[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(4): 448~450
赖莺,董清木,林睿,葛秀秀,蔡延平,林海霞. 超高效液相色谱-质谱法测定环氧树脂粘结剂中双酚A[J]. 理化检验-化学分册, 2013, 49(4): 448~450
被引情况:
【1】凌绍明,欧阳辉祥,黄宝敬, "基于固绿褪色反应的分光光度法测定双酚A的含量",理化检验-化学分册 52, 625-628(2016)
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参考文献
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【3】李鱼,刘建林,王晓丽,等.分散液液微萃取-高效液相色谱法测定水样中的痕量双酚A[J].高等学校化学学报, 2008,29(11):2142-2148.
【4】杨红梅,王浩,刘艳琴,等.液相色谱-串联三重四极杆质谱测定饮料中双酚A残留[J].食品研究与开发, 2009,30(12):137-139.
【5】黄少婵,杭义萍.液相色谱-质谱法同时测定塑料制品中双酚A和四溴双酚A[J].色谱, 2010,28(9):863-866.
【6】蔡亚岐,江桂斌,周庆祥.胶束电动色谱法分离和测定双酚A、辛基酚和壬基酚[J].分析化学, 2004,32(9):1179-1181.
【7】SHIN Ho-sang, PARK Chi-hu, PARK Song-ja, et al. Sensitive determination of bisphenol A in evironmental water by gas chromatography with nitroge/phosphorus detection after cyanomethylation[J]. Journal of Chromatography A, 2001,912:119-125.
【8】GEENS T, NEELS H, COVACI A. Sensitive and selective method for the determinatio of bisphenol-A and triclosan I serum and urine as petafluorobenzoate-derivatives using GC/ECNI/MS[J]. Journal of Chromatography B, 2009,877:4042-4046.
【9】魏孔吉,赵美萍,李元宗,等.生物素-亲和素放大酶联免疫吸附法测定双酚A[J].分析化学, 2005,33(8):1122-1124.
【10】张宏,郭大城,孙成均.示波极谱法测定聚碳酸酯塑料中双酚A[J].理化检验-化学分册, 2002,38(8):379-381.
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