Determination of endocrine disrupting compounds in fish liver, brain, and muscle using focused ultrasound solid–liquid extraction and dispersive solid phase extraction as clean-up strategy
Determination of endocrine disrupting compounds in fish liver, brain, and muscle using focused ultrasound solid–liquid extraction and dispersive solid phase extraction as clean-up strategy
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DOI：
10.1007/s00216-016-9697-3
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发表时间：
2016-06
影响因子：
4.3
通讯作者：
O. Ros;A. Vallejo;M. Olivares;N. Etxebarria;A. Prieto
中科院分区：
文献类型：
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作者：
O. Ros;A. Vallejo;M. Olivares;N. Etxebarria;A. Prieto
本研究描述了一种新的方法，同时提取几种内分泌干扰物，包括烷基酚（AP），雌激素，双酚A（BPA）和一个邻苯二甲酸酯代谢产物（单-2-乙基己基酯，MEHP）在鱼的肝脏，脑，肌肉。评价了影响浸提（浸提溶剂和温度）和清洁（分散相性质和量）步骤的参数。通过聚焦超声固液萃取（FUSLE），使用10 mL正己烷：丙酮（50：50，v/v）在约0 ℃下进行5 min的萃取，并通过分散固相萃取（dSPE）进行净化，使用100 mg NH_4CARB和100 mg MgSO 4清洗脑和肌肉提取物，在肝脏提取物的情况下使用100 mg PSA。在肝脏（62- 132%）、脑（66- 120%）和肌肉（74- 129%）中获得了良好的表观回收率，相对标准偏差（RSD%）始终低于26%，方法检测限（MDLs）处于低ng/g水平。开发的方法应用于2015年12月在Urdaibai河口（比斯开湾）捕获的鱼类，获得的浓度范围为大脑中的MDL-1115 ng/g，肌肉中的MDL-962 ng/g和肝脏中的MDL-672 ng/g。一般而言，在肝脏中测得的浓度最高，其次是大脑和肌肉。另外，己烯雌酚仅在鱼脑中被检测到。图示摘要MS方法方案为/MS方法方案用于鱼肝、脑和肌肉中内分泌干扰物的测定
This study describes a new method for the simultaneous extraction of several endocrine disrupting compounds, including alkylphenols (APs), estrogen, bisphenol-A (BPA) and one phthalate metabolite (mono-2-ethylhexyl ester, MEHP) in fish liver, brain, and muscle. Parameters affecting the extraction (extraction solvent and temperature) and the clean-up (dispersive phase nature and amount) steps were evaluated. The extraction was performed by means of focused ultrasound solid–liquid extraction (FUSLE) using 10 mL ofn-hexane:acetone (50:50, v/v) for 5 min at ~0 °C, and the clean-up was done by means of dispersive solid phase extraction (dSPE) using 100 mg of ENVI-CARB and 100 mg of MgSO4for the cleaning of brain and muscle extracts together with 100 mg of PSA in the case of liver extracts. Good apparent recoveries were obtained in the case of liver (62–132 %), brain (66–120 %), and muscle (74–129 %), relative standard deviation (RSD%) was always below 26 %, and the method detection limits (MDLs) were at low ng/g level. The developed method was applied to fish captured in Urdaibai estuary (Bay of Biscay) in December 2015, and the concentrations obtained were in the range MDL-1115 ng/g in brain, MDL-962 ng/g in muscle, and MDL-672 ng/g in liver. In general, the highest concentrations were measured in liver, followed by brain and muscle. In addition, diethylstilbestrol was only detected in fish brain.Graphical AbstractMS method scheme for the/MS method scheme for the determination of EDCs in fish liver, brain and muscle