分散液液微萃取-超高效液相色谱-串联质谱法快速测定市售饮用水样中7种双酚-二环氧甘油醚
Rapid determination of seven bisphenol diglycidyl ethers in drinking water samples by dispersive liquid-liquid microextraction-ultra high performance liquid chromatography-tandem mass spectrometry
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摘要: 基于分散液液微萃取技术，以实际样品为研究对象，建立了饮用水中内分泌干扰物双酚A-二缩水甘油醚（BADGE）及其衍生物（BADGE·H2O、BADGE·2H2O、BADGE·HCl、BADGE·2HCl、BADGE·H2O·HCl）和双酚F-二缩水甘油醚（BFDGE）等7种双酚-二环氧甘油醚的分散液液微萃取-超高效液相色谱-串联质谱（DLLME-UPLC-MS/MS）检测方法.以三氯甲烷作为萃取剂（3.00 mL）、丙酮为分散剂（2.00 mL）制备分散液液微萃取系统，超声辅助萃取和浓缩样品中的双酚-二环氧甘油醚.含有0.01 mol·L-1乙酸铵和1%甲酸的甲醇水溶液作为流动相，Waters Symmetry® C18分离后，电喷雾正离子（ESI+）模式串联四极杆质谱检测.7种双酚-二环氧甘油醚在5.0-1000.0 μg·L-1范围内线性关系良好，相关系数均大于0.9953；在50.00、100.00 μg·L-1和500.00 μg·L-1的3个添加水平下，7种目标化合物的平均回收率为79.9%-100.7%，相对标准偏差（RSD）均低于11.6%，检出限在0.5-5.0 μg·L-1.该方法操作简单，灵敏度高，重复性好，能够在9 min内实现7种双酚-二环氧甘油醚的快速检测和定量分析.
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关键词:
- 分散液液微萃取 /
- 超高效液相色谱-串联质谱法 /
- 双酚-二环氧甘油醚 /
- 饮用水 /
- 内分泌干扰物
Abstract: A method based on dispersive liquid-liquid microextraction-ultra high performance liquid chromatography-tandem mass spectrometry (DLLME-UPLC-MS/MS) was developed for the rapid determination of seven bisphenol diglycidyl ethers (BADG, BADGE·H2O, BADGE·2H2O, BADGE·HCl, BADGE·2HCl, BADGE·H2O·HCl, BFDGE) in drinking water samples. The samples in the study were extracted with DLLME method, in which the extraction solvent and dispersive solvent were CHCl3 (3.00 mL) and acetone (2.00 mL), respectively, by ultrasonic wave assisted extraction. The separation was performed on Waters Symmetry® C18 column with a methanol solution consisting of 0.01 mol·L-1 ammonium acetate and 1% formic acid. The targeted compounds were analyzed by UPLC-MS/MS with the multiple reaction monitoring (MRM) mode. All the seven bisphenol diglycidyl ethers showed good linearity in the range of 5.0-1000.0 μg·L-1, with the correlation coefficients (R2) higher than 0.9953. At three concentrations (50.00, 100.00 and 500.00 μg·L-1), the average recoveries were in the range of 79.9%-100.7% and the RSDs were less than 11.6%. The limits of detection of the method were between 0.5 to 5.0 μg·L-1. The method has the advantages of high sensitivity, simplicity and reliability, which takes just 9 min to detect bisphenol diglycidyl ethers in drinking water samples. -
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