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同时测定贻贝中天然雌激素和非甾体抗炎药。

Simultaneous determination of non-steroidal anti-inflammatory drugs and natural estrogens in the mussels Mytilus edulis trossulus.

机构信息

Department of Environmental Analysis, Faculty of Chemistry, University of Gdansk, Wita Stwosza 63, 80-308 Gdańsk, Poland.

Institute of Oceanology, Polish Academy of Sciences, Powstańców Warszawy 55, 81-712 Sopot, Poland.

出版信息

Talanta. 2019 Aug 1;200:316-323. doi: 10.1016/j.talanta.2019.03.062. Epub 2019 Mar 15.

Abstract

In this study, an ASE (Accelerated Solvent extraction)-SPE (Solid Phase Extraction)-GC/MS(SIM) method for the simultaneous determination of five non-steroidal anti-inflammatory drugs (NSAIDs: ibuprofen (IBU), paracetamol (PAR), diclofenac (DIC), naproxen (NAP) and ketoprofen (KET)) and three natural estrogens (estrone (E1), 17β-estradiol (E2), estriol (E3)) in mussels was proposed, which is simple, cheap and easy for use in environmental laboratories. For the first time, the sorbents: PSA (Primary Secondary Amine) and FLORISIL®, placed directly inside the extraction cells, were used for the improvement of the ASE procedure for the isolation of these pollutants from mussel samples. The application of FLORISIL® especially allowed the purification of the extract to increase recovery, without the loss of analytes, or prolongation of the extraction time. The proposed ASE-SPE-GC/MS(SIM) method was validated (the method detection limit values were in the range of 1 ng/g dry weight (d.w.) for IBU to 7 ng/g d.w. for E1; the measurement intermediate precision was between 0.24% and 7.85%; the mean recovery was in the range of 80-118%) and used for the determination of NSAIDs and estrogenic hormones in whole tissue of the mussels Mytilus edulis trossulus collected from the Gulf of Gdansk (southern Baltic Sea). IBU, NAP, DIC and E1 were determined in these samples; however, the pharmaceuticals were found only in smaller (with a length of 2-3 cm) individuals. The observed differences in the concentrations of CEC in smaller and older mussel organisms were fully discussed. Summarizing, this method could be used for monitoring these CEC in such organisms in order to expand our knowledge of their influence on the water ecosystem, however, in such investigations smaller mussel organisms should be used.

摘要

本研究提出了一种 ASE(加速溶剂萃取)-SPE(固相萃取)-GC/MS(SIM)方法,用于同时测定贻贝中五种非甾体抗炎药(NSAIDs:布洛芬(IBU)、扑热息痛(PAR)、双氯芬酸(DIC)、萘普生(NAP)和酮洛芬(KET))和三种天然雌激素(雌酮(E1)、17β-雌二醇(E2)、雌三醇(E3))。该方法简单、廉价,易于在环境实验室中使用。首次将 PSA(伯仲胺)和 Florisil®直接置于萃取池内,作为 ASE 程序的改进,用于从贻贝样品中分离这些污染物。Florisil®的应用尤其允许对提取物进行净化,以提高回收率,而不会损失分析物或延长提取时间。所提出的 ASE-SPE-GC/MS(SIM)方法经过验证(方法检测限范围为 1ng/g 干重(d.w.)的 IBU 至 7ng/g d.w.的 E1;测量中间精密度在 0.24%-7.85%之间;平均回收率在 80%-118%之间),并用于测定从加里宁格勒湾(波罗的海南部)采集的贻贝 Mytilus edulis trossulus 全组织中的 NSAIDs 和雌激素。在这些样品中测定了 IBU、NAP、DIC 和 E1;然而,只在较小(长度为 2-3cm)的个体中发现了这些药物。充分讨论了较小和较老的贻贝生物中 CEC 浓度的差异。综上所述,该方法可用于监测这些 CEC 在这些生物体中的存在,以扩大我们对其对水生态系统影响的认识,然而,在这种调查中,应使用较小的贻贝生物体。

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