色谱

色谱 ›› 2012, Vol. 30 ›› Issue (10): 1002-1007.DOI: 10.3724/SP.J.1123.2012.08024

• 专栏 • 上一篇    下一篇

高效液相色谱-串联质谱法同时测定肉类罐头中双酚-二缩水甘油醚

赵晓亚*, 付晓芳, 王鹏, 李晶, 胡小钟   

  1. 湖北出入境检验检疫局技术中心, 湖北 武汉 430050
  • 收稿日期:2012-08-16 修回日期:2012-09-10 出版日期:2012-10-28 发布日期:2012-10-17
  • 通讯作者: 赵晓亚,博士,高级工程师,主要从事食品、化妆品安全及检测研究. Tel: (027)58906069, E-mail: zhaoxy@hbciq.gov.cn.
  • 基金资助:

    国家质量监督检验检疫总局检验检疫行业标准(2008B173).

Determination of bisphenol diglycidyl ether residues in canned foodstuffs by high performance liquid chromatography-tandem mass spectrometry

ZHAO Xiaoya*, FU Xiaofang, WANG Peng, LI Jing, HU Xiaozhong   

  1. Hubei Entry-Exit Inspection and Quarantine Bureau, Wuhan 430050, China
  • Received:2012-08-16 Revised:2012-09-10 Online:2012-10-28 Published:2012-10-17

PDF

466

被引次数

16

摘要： 建立了同时测定肉类罐头中双酚A-二缩水甘油醚(BADGE)、双酚F-二缩水甘油醚(BFDGE)及其衍生物双酚A-(2,3-二羟丙基)甘油醚(BADGE•H2O)、双酚A-双(2,3-二羟丙基)醚(BADGE•2H2O)、双酚A-(3-氯-2-羟丙基)(2,3-二羟丙基)醚(BADGE•H2O•HCl)、双酚A-(3-氯-2-羟丙基)甘油醚(BADGE•HCl)、双酚A-双(3-氯-2-羟丙基)醚(BADGE•2HCl)、双酚F-双(2,3-二羟丙基)醚(BFDGE•2H2O)、双酚F-双(3-氯-2-羟丙基)醚(BFDGE•2HCl)9种环境激素的高效液相色谱-串联质谱分析方法。样品经叔丁基甲醚提取,HLB固相萃取小柱净化,C18色谱柱分离,用5 mmol/L醋酸铵溶液(含0.1%甲酸)与甲醇为流动相梯度洗脱,质谱多反应监测(MRM)模式检测,基质标准校正,外标法定量。结果表明,这9种化合物在10.0～2000.0 μg/L范围内线性关系良好;定量限(以信噪比≥10计)为10.0 μg/kg;在高、中、低3个加标水平下9种化合物的平均添加回收率为79.6%～100.9%,相对标准偏差为6.3%～12.1%。该方法具有较高的灵敏度和准确度,能满足法规要求的对肉类罐头中双酚A-二缩水甘油醚、双酚F-二缩水甘油醚及其衍生物残留量的快速检测及准确定量。

关键词: 高效液相色谱-串联质谱, 肉类罐头, 双酚-二缩水甘油醚

Abstract: An accurate quantitative determination and confirmative method for bisphenol diglycidyl ether residues, bisphenol A diglycidyl ether (BADGE), bisphenol F diglycidyl ether (BFDGE), bisphenol A (2,3-dihydroxypropyl)glycidyl ether (BADGE•H2O), bisphenol A bis(2,3-dihydroxypropyl) ether (BADGE•2H2O), bisphenol A (3-chloro-2-hydroxy propyl)(2,3- dihydroxypropyl) ether (BADGE•H2O•HCl), bisphenol A (3-chloro-2-hydroxypropyl)glycidyl ether (BADGE•HCl), bisphenol A bis(3-chloro-2-hydroxypropyl) ether (BADGE•2HCl), bisphenol F bis(2,3-dihydroxypropyl) ether (BFDGE•2H2O), bisphenol F bis(3-chloro-2-hydroxypropyl) ether (BFDGE•2HCl) in canned foodstuffs by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has been established. The sample was extracted with tert-butylmethyl ether and the extract was cleaned-up and concentrated on a Waters Oasis HLB column. The target compounds were analyzed by HPLC-MS/MS on a C18 column by the gradient elution with methanol and 5 mmol/L ammonium acetate containing 0.1% formic acid in a multiple reaction monitoring (MRM) scan mode. External matrix standard solutions were used for the quantitative determination and the calibration curves showed good linearity in the concentration range of 10.0~2000.0 μg/L for the nine target compounds. The limits of quantification of the nine compounds were 10.0 μg/kg (S/N≥10). The average recoveries of the nine compounds ranged from 79.6% to 100.9% at the spiked levels of 10.0, 100.0, 1000.0 μg/kg with the relative standard deviations (RSDs) of 6.3%~12.1%. The method is sensitive, accurate, and suitable for the rapid determination of bisphenol diglycidyl ether residues in canned foodstuffs.

Key words: bisphenol diglycidyl ethers, canned foodstuffs, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)