固相萃取-高效液相色谱-串联质谱测定水中8种双酚-二环氧甘油醚

Determination of eight bisphenol diglycidyl ethers in water bysolid phase extraction-highperformance liquid chromatography-tandem mass spectrometry

建立了水中8种双酚-二环氧甘油醚（双酚A二缩水甘油醚（BADGE）及其衍生物双酚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·HCl·H2O）和双酚F-二环氧甘油醚（BFDGE）及其衍生物双酚F双（3-氯-2-羟丙基）醚（BFDGE·2HCl））的固相萃取-高效液相色谱-串联质谱（SPE-HPLC-MS/MS）测定方法。10个饮用水接触涂料样品在室温避光条件下,以超纯水浸泡（24±1）h,然后取200 mL经C18固相萃取柱进行净化浓缩,以C18色谱柱进行分离,以5 mmol/L醋酸铵、甲醇和水为流动相进行梯度洗脱,质谱多反应监测（MRM）模式检测,外标法定量。结果表明,8种双酚-二环氧甘油醚在0.007-5.00μg/L线性关系良好,相关系数均大于0.999 0,该方法对8种双酚-二环氧甘油醚的定量限为7-91ng/L,回收率为79.1%-101%,RSD为4.0%-12%。该方法具有灵敏度高、选择性强的特点,能够满足水中双酚-二环氧甘油醚的快速检测和准确定量。

A solid phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry（SPE-HPLC-MS/MS）method was developed for the determination of eight bisphenol diglycidyl ethers,including bisphenol A diglycidyl ether（BADGE）,bisphenol A（3-chloro-2-hydroxypropyl）glycidyl ether（BADGE·HCl）,bisphenol A bis（3-chloro-2-hydroxypropyl）ether（BADGE·2HCl）,bisphenol A（2,3-dihydroxypropyl）glycidyl ether（BADGE·H2O）,bisphenol A bis（2,3-dihydroxypropyl）ether（BADGE·2H2O）,bisphenol A（3-chloro-2-hydroxypropyl）（2,3-dihydroxypropyl）ether（BADGE·HCl·H2O）,bisphenol F diglycidyl ether（BFDGE）and bisphenol F bis（3-chloro-2-hydroxypropyl）ether（BFDGE·2HCl）in water.A total of ten samples were collected from the leaching of the coatings for drinking water supply system.Then,200 mL exposure water was preconcentrated on C18solid-phase extraction cartridge.The eight compounds were analyzed by liquid chromatography-tandem mass spectrometry method on a C18column by the gradient elution with methanol,water and 5 mmol/L ammonium acetate as mobile phases in the multiple reaction monitoring（MRM）scan mode.The external matrix standard solutions were used for the quantitative determination and the calibration curves of the eight compounds showed good linearity in the range of 0.007-5.00μg/L with the correlation coefficients more than0.999 0.The limits of quantification（LOQs）of the method were 7-91 ng/L.The spiked recov-eries ranged from79.1%to 101% with the relative standard deviations of 4.0%-12%.The method is sensitive and accurate,and is applicable to the determination of bisphenol diglycidyl ethers in water.