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Simultaneous determination of triazine herbicides and their metabolites in shellfish by HPLC-MS/MS combined with Q/E-Orbitrap HRMS

文献类型： 外文期刊

作者： Sun, Xiaojie 1 ; Gao, Jinfang 3 ; Xing, Jun 4 ; Xing, Lihong 1 ; Guo, Mengmeng 1 ; Peng, Jixing 1 ; Li, Zhaoxin 1 ; Tan, 1 ;

作者机构： 1.Minist Agr & Rural Affairs, Key Lab Testing & Evaluat Aquat Prod Safety & Qua, Qingdao 266071, Shandong, Peoples R China

2.Chinese Acad Fishery Sci, Yellow Sea Fisheries Res Inst, Qingdao 266071, Shandong, Peoples R China

3.Weifang Inst Inspect Prod Qual, Weifang 266000, Peoples R China

4.Wuhan Univ, Coll Chem & Mol Sci, Key Lab Analyt Chem Biol & Med, Minist Educ, Wuhan 430072, Hubei, Peoples R China

关键词： Triazine herbicides; Metabolites; Shellfish; HPLC-MS/MS; Q/E-Orbitrap HRMS

期刊名称：ANALYTICAL AND BIOANALYTICAL CHEMISTRY （ 影响因子：4.157； 五年影响因子：3.868 ）

ISSN： 1618-2642

年卷期： 2021 年 413 卷 25 期

页码：

收录情况： SCI

摘要： Triazine herbicides are used extensively in agriculture and aquaculture worldwide because of their broad effectiveness in weed control. However, after they are discharged into the sea, they seriously contaminate aquatic ecosystems and threaten aquatic organisms, especially shellfish. Currently, there are no established methods for the detection and confirmation of triazine herbicides and their metabolites in biological matrixes. Hence, the food safety of aquatic products cannot be accurately evaluated, which creates a technical barrier against international aquatic product trade. In this study, for the first time, a method was developed for the analysis and confirmation of seven triazine herbicides and 13 metabolites in shellfish, based on alkaline acetonitrile extraction and neutral Al2O3 cartridge purification coupled with internal standard calibration. Specifically, quantitative and qualitative analysis was conducted using high-performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS), and accurate identification was carried out by quadrupole orbitrap high-resolution mass spectrometry (Q/E Orbitrap HRMS). The results showed that target analytes demonstrated good linearity within the corresponding range (R-2 > 0.995). The limit of detection and limit of quantitation of the proposed method were 0.1 and 0.3 mu g/kg, respectively. The average recoveries of analytes were between 70.0% and 120% when spiked at three levels with blank oyster (Crassostrea gigas) as the matrix, and the relative standard deviations (RSDs) were all less than 12% (n=6). The proposed method was successfully applied for the detection of triazine herbicide residues in oyster samples during actual breeding, and the presence of DIP, HP, DEHA, and other metabolites in positive samples was confirmed by Q/E Orbitrap HRMS. This method exhibits high accuracy, high sensitivity, and good reproducibility. It has promising application prospects in the field of hazard analysis and the positive identification of aquatic products.

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