Alvarez-Muñoz D, Huerta B, Fernandez-Tejedor M, Rodríguez-Mozaz S, Barceló D
Catalan Institute for Water Research (ICRA), Parc Científic i Tecnològic de la Universitat de Girona, C/Emili Grahit, 101 Edifici H2O, E-17003 Girona, Spain.
Institute of Agriculture and Food Research and Technology (IRTA), Ctra. Poble Nou, km 5.5, Sant Carles de la Ràpita, Tarragona 43540, Spain.
Talanta. 2015 May;136:174-82. doi: 10.1016/j.talanta.2014.12.035. Epub 2014 Dec 30.
A fast, simple and robust method has been developed for the simultaneous determination of 23 pharmaceuticals (including some major metabolites) in bivalve mollusks. The analytes belong to eight different therapeutic groups: antibiotics, psychiatric drugs, analgesics/anti-inflammatories, tranquilizer, calcium channel blockers, diuretic, and prostatic hyperplasia. The method is based on pressurized liquid extraction (PLE) followed by solid phase extraction clean-up (SPE), and ultra performance liquid chromatography-triple quadrupole mass spectrometry (UHPL-MS/MS) for the identification and quantification of the target analytes. It has been developed and validated in three different species of bivalves: Crassostrea gigas (Pacific oyster), Mytilus galloprovincialis (Mediterranean mussel), and Chamelea gallina (striped venus clam). The majority of the compounds were extracted with a recovery between 40 and 115%. The developed analytical method allowed the determination of the compounds in the lower ng/g concentration levels. The relative standard deviation was under 12% for the intra-day and 20% inter-day analyses, respectively. Finally, the method was applied to oyster, clam and mussel samples collected from the Ebro delta, Spain. The most ubiquitous compounds detected were the psychiatric drug venlanfaxine and the antibiotic azithromycin, with the highest concentrations found in mussel (2.7ng/g dw) and oyster (3.0ng/g dw), respectively. To the best of our knowledge, this is the first time that azithromycin has been reported in environmental samples of marine biota.
已开发出一种快速、简便且稳健的方法，用于同时测定双壳贝类软体动物中的23种药物（包括一些主要代谢物）。这些分析物属于八个不同的治疗类别：抗生素、精神药物、镇痛药/抗炎药、镇静剂、钙通道阻滞剂、利尿剂和前列腺增生药物。该方法基于加压液体萃取（PLE），随后进行固相萃取净化（SPE），并采用超高效液相色谱-三重四极杆质谱联用仪（UHPL-MS/MS）对目标分析物进行鉴定和定量。该方法已在三种不同的双壳贝类中开发并验证：太平洋牡蛎（Crassostrea gigas）、地中海贻贝（Mytilus galloprovincialis）和条纹维纳斯蛤（Chamelea gallina）。大多数化合物的萃取回收率在40%至115%之间。所开发的分析方法能够测定浓度低至纳克/克水平的化合物。日内分析的相对标准偏差低于12%，日间分析的相对标准偏差低于20%。最后，该方法应用于从西班牙埃布罗三角洲采集的牡蛎、蛤和贻贝样本。检测到的最普遍存在的化合物是精神药物文拉法辛和抗生素阿奇霉素，在贻贝（2.7纳克/克干重）和牡蛎（3.0纳克/克干重）中分别发现了最高浓度。据我们所知，这是首次在海洋生物群的环境样本中报道阿奇霉素。
