浙江农业学报 ›› 2025, Vol. 37 ›› Issue (3): 689-700.DOI: 10.3969/j.issn.1004-1524.20240352

• 农产品质量安全 • 上一篇    下一篇

基于响应面分析的养殖水产品中高风险喹诺酮类抗生素残留及其基质效应研究

徐汇镔1,2,3(), 朱洁1,2,3,*(), 周朝生1,2,3, 胡园1,2,3, 陆荣茂1,2,3   

  1. 1.浙江省海洋水产养殖研究所,浙江 温州 325005
    2.浙江省近岸水域生物资源开发与保护重点实验室,浙江 温州 325005
    3.全省近岸生物种质资源保护与利用重点实验室,浙江 温州 325005
  • 收稿日期:2024-04-16 出版日期:2025-03-25 发布日期:2025-04-02
  • 作者简介:徐汇镔(1994—),男,浙江温州人,学士,助理工程师,从事水产养殖及水产品质量安全研究工作。E-mail:361233617@qq.com
  • 通讯作者: * 朱洁,E-mail:441871423@qq.com
  • 基金资助:
    浙江省基础公益研究计划(LTGC23B050007)

Study for the determination of high-risk quinolone antibiotics residues and its matrix effect in cultured aquatic products by UPLC-MS/MS based on response surface analysis

XU Huibin1,2,3(), ZHU Jie1,2,3,*(), ZHOU Chaosheng1,2,3, HU yuan1,2,3, LU Rongmao1,2,3   

  1. 1. Zhejiang Mariculture Research Institute, Wenzhou 325005, Zhejiang, China
    2. Zhejiang Key Laboratory of Exploitation and Preservation of Coastal Bio-Resource, Wenzhou 325005, Zhejiang, China
    3. Zhejiang Key Laboratory of Coastal Biological Germplasm Resources Conservation and Utilization, Wenzhou 325005, Zhejiang, China
  • Received:2024-04-16 Online:2025-03-25 Published:2025-04-02

摘要:

为建立大黄鱼、鲫鱼、中华鳖等大宗养殖水产品中高风险喹诺酮类抗生素的通用、高效、准确的残留分析方法,利用超声振荡联用法对目标物进行提取,经液液萃取完成净化并采用UPLC-MS/MS测定。通过提取试剂中的酸含量、振荡时间、超声时间、氮吹压力、温度等变量结合Box-Behnken响应面分析确定最优前处理条件。同时评价大黄鱼、鲫鱼、中华鳖、南美白对虾、青蟹及其性腺、缢蛏中目标物的基质效应,并通过同位素内标、基质匹配曲线探讨了基质效应的补偿途径。结果表明:6种目标物的平均回收率为82.20%~118.00%;在0.2~20 ng·mL-1线性范围内,线性相关系数均大于0.997,氧氟沙星、洛美沙星、诺氟沙星、培氟沙星、环丙沙星检出限为0.1 μg·kg-1,恩诺沙星检出限为0.5 μg·kg-1,定量限均为1.0 μg·kg-1。该方法满足水产品中喹诺酮类残留的检测要求。南美白对虾、青蟹性腺、大黄鱼基质对6种目标物均有不同程度的抑制作用,基质匹配曲线和内标法均可使基质效应得到有效补偿。

关键词: 响应面分析, 超高效液相色谱串联质谱, 养殖水产品, 高风险, 喹诺酮, 基质效应评价

Abstract:

In order to establish an general, efficient and accurate residue analysis method for high risk quinolone antibiotics in cultured aquatic products, such as Larimichthys crocea, Carassius auratus, Pelodiscus sinensis, etc, all the samples were extracted using ultrasonic and vibrating extraction coupling, and then cleaned by liquid-liquid extraction and determined by UPLC-MS/MS. The optimal pretreatment conditions were determined by combining hydrochloric acid concentration in extraction reagent, oscillation time, ultrasonic time, nitrogen blowing pressure, temperature with Box-Behnken response surface analysis. The matrix effects of the target objects were evaluated in this study, and the compensation method of matrix effects in Larimichthys crocea, Carassius auratus, Pelodiscus sinensis, Penaeus vannemei, Scylla serrata and its gonad, and Sinonovacula constricta was discussed by isotope internal standard and matrix matching curve. The results showed that the average recovery rate of 6 target substances was 82.20%-118.00%. The linear correlation coefficients were above 0.997 in spiked range of 0.2-20 ng·mL-1. The limits of detection and limits of quantitation were 0.5 μg·kg-1 and 1.0 μg·kg-1, respectively. It showed that the method met the requirements for the analysis of antibiotic residues in cultured aquatic products. To varying degrees, the matrix of Penaeus vannamei, Scylla serrata gonad and Larimichthys crocea inhibited the 6 target substances. The matrix matching curve and internal standard method could compensate the matrix effect effectively.

Key words: response surface, UPLC-MS/MS, cultured aquatic product, high risk, quinolone, matrix effects evaluation

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