Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080, Bilbao, Spain.
Research Centre for Experimental Marine Biology and Biotechnology (PIE), University of the Basque Country (UPV/EHU), Areatza z/g, 48620, Plentzia, Spain.
Anal Bioanal Chem. 2019 Jan;411(2):493-506. doi: 10.1007/s00216-018-1474-z. Epub 2018 Nov 26.
In this work, the full optimisation and validation procedure to analyse a wide set of emerging organic contaminants in biotissues (mussel and fish muscle, liver, gills and brain) and biofluids (fish plasma and bile) is described. The target families include artificial sweeteners, industrial products, hormones, pharmaceutical and personal care products, pesticides and phytoestrogens. Different clean-up strategies (hydrophilic-lipophilic-balanced (HLB) solid-phase extraction, Florisil solid-phase extraction and liquid-liquid extraction followed by HLB solid-phase extraction and microextraction based on polyethersulfone polymer) were evaluated for the clean-up of focused ultrasonic solid-liquid extraction (FUSLE) extracts before the analysis by liquid chromatography-triple quadrupole tandem mass spectrometry (LC-QqQ-MS/MS). The methods afforded satisfactory apparent recovery values (71-126%) using isotopically labelled analytes and matrix-matched calibration approach, regardless of the matrix. Method detection limits in the range of 4-48 ng/g and 0.3-111 ng/L were obtained for biotissues and biofluids, respectively. The developed method was applied to determine the uptake and tissue distribution in juvenile gilt-head bream (Sparus aurata) during 7 days in seawater, and unexpectedly, perfluoro-1-butanesulfonate tended to accumulate in liver and, to a lesser extent, in muscle and gills. Furthermore, real mussel samples collected in the Basque coast were also analysed and the presence of the highly consumed valsartan (7 ng/g) and telmisartan (6.8 ng/g) compounds in bivalves is reported for the first time here. Graphical abstract ᅟ.
本工作描述了一种广泛用于分析生物组织（贻贝和鱼肉、肝脏、鳃和脑）和生物体液（鱼类血浆和胆汁）中新兴有机污染物的全优化和验证程序。目标家族包括人工甜味剂、工业产品、激素、药物和个人护理产品、农药和植物雌激素。针对不同的净化策略（亲水-亲脂平衡固相萃取（HLB）、Florisil 固相萃取和液液萃取后采用 HLB 固相萃取和基于聚醚砜聚合物的微萃取）进行了评估，用于聚焦超声固液萃取（FUSLE）提取物的净化，然后采用液相色谱-三重四极杆串联质谱（LC-QqQ-MS/MS）进行分析。该方法使用同位素标记的分析物和基质匹配校准方法，无论基质如何，都能获得令人满意的表观回收率值（71-126%）。生物组织和生物体液的方法检测限分别为 4-48 ng/g 和 0.3-111 ng/L。该方法应用于研究幼金头鲷（Sparus aurata）在海水中 7 天内的吸收和组织分布情况，出人意料的是，全氟-1-丁烷磺酸盐倾向于在肝脏中积累，在肌肉和鳃中积累程度较小。此外，还对巴斯克海岸采集的真实贻贝样本进行了分析，并首次报道了在双壳类动物中存在高消耗的缬沙坦（7 ng/g）和替米沙坦（6.8 ng/g）化合物。
