食品科学 ›› 2020, Vol. 41 ›› Issue (18): 258-266.doi: 10.7506/spkx1002-6630-20190903-035

• 安全检测 • 上一篇    下一篇

QuEChERS结合UPLC-MS/MS测定水产品中9 种除草剂残留及基质效应

李丽春,刘书贵,尹怡,汪玉洁,郑光明,马丽莎,单奇,戴晓欣,赵城,谢文平,魏琳婷   

  1. (1.中国水产科学研究院珠江水产研究所,农业农村部水产品质量安全风险评估实验室(广州),农业农村部休闲渔业重点实验室,广东?广州 510380;2.仲恺农业工程学院,广东?广州 510225)
  • 出版日期:2020-09-25 发布日期:2020-09-18
  • 基金资助:
    国家自然科学基金青年科学基金项目(31501398); 中国水产科学研究院中央级公益性科研院所基本科研业务费专项(2017HY-ZC0603); 国家水产品质量安全风险评估项目(GJFP201800902)

Determination of Nine Herbicide Residues in Aquatic Products Using QuEChERS Combined with UPLC-MS/MS and Evaluation of Matrix Effects

LI Lichun, LIU Shugui, YIN Yi, WANG Yujie, ZHENG Guangming, MA Lisha, SHAN Qi, DAI Xiaoxin, ZHAO Cheng, XIE Wenping, WEI Linting   

  1. (1. Laboratory of Quality & Safety Risk Assessment for Aquatic Product (Guangzhou), Key Laboratory of Recreational Fisheries Research, Ministry of Agriculture and Rural Affairs, Pearl River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Guangzhou 510380, China; 2. Zhongkai University of Agriculture and Engineering, Guangzhou 510225, China)
  • Online:2020-09-25 Published:2020-09-18

摘要: 建立水产品中9?种除草剂(扑草津、乙草胺、丁草胺、二氯喹啉酸、苄嘧磺隆、甲磺隆、莠去津、利谷隆和灭草松)残留的QuEChERS结合超高效液相色谱-串联质谱检测方法。采用多反应监测正离子模式测定,以外标法定量,分析9?种除草剂的基质效应及其影响因素。结果表明:9?种除草剂在0.50~100?ng/mL(二氯喹啉酸和利谷隆为1.00~100?ng/mL)质量浓度范围内线性关系良好,相关系数(r)大于0.99,方法检出限和定量限分别为0.20~0.50?μg/kg和0.50~1.50?μg/kg。在对虾、鲤鱼、鲫鱼和鳙鱼空白基质中平均加标回收率为84.33%~116.37%(n=6),精密度为0.80%~13.81%(n=6),该方法适用于水产品中9?种除草剂残留量的测定。该方法下基质种类、基质质量和除草剂质量浓度对基质效应有一定影响,二氯喹啉酸、甲磺隆和苄嘧磺隆在鲤鱼和对虾中均存在较强的基质增强效应,丁草胺、乙草胺、利谷隆、灭草松和莠去津在4?种水产品基质中均表现为基质抑制效应。在实际检测水产品中除草剂残留时,应采用基质校准曲线减弱基质效应确保检测结果的准确性。

关键词: QuEChERS;超高效液相色谱-串联质谱;水产品;除草剂;基质效应

Abstract: A quick, easy, cheap, effective, rugged, and safe (QuEChERS) combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for determination of 9 herbicide residues (prometryn, acetochlor, butachlor, quinclorac, bensulfuron methyl, metsulfuron methyl, atrazine, linuron and bentazone) in aquatic products. Detection was carried out in the positive ion mode with multiple reaction monitoring and the external standard method was used for quantification. The matrix effects in the determination of the nine herbicides and the factors influencing?them were analyzed. The results showed that good linearity was observed for quinclorac and linuron in the concentration range of 1.00–100 ng/mL and for seven other herbicides in the concentration range of 0.50–100 ng/mL with correlation coefficients above 0.99. The limits of detection (LODs) and limits of quantitation (LOQs) for all herbicides were in the ranges of 0.20–0.50 and 0.50–1.50 μg/kg, respectively. The average recoveries of the herbicides spiked into blank samples of Penaeus orientalis, Cyprinus carpio, Carassius auratus and Aristichthys nobilis were 84.33%–116.37% (n = 6), and the precision expressed as relative standard deviation (RSD) was 0.80%–13.81% (n = 6). This method could be applied to determine the 9 herbicide residues in aquatic products. The type and mass of matrix and herbicide concentration influenced the matrix effect. Quinclorac, bensulfuron methyl and metsulfuron methyl showed strong matrix enhancement effects in P. orientalis and C. carpio, while butachlor, acetochlor, linuron, bentazone and atrazine showed matrix inhibition effects in all four aquatic products. The matrix calibration curve should be used to reduce the matrix effects to ensure the accuracy in the detection of herbicide residues in aquatic products.

Key words: QuEChERS; ultra-high performance liquid chromatography-tandem mass spectrometry; aquatic products; herbicides; matrix effects

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