食品科学 ›› 2025, Vol. 46 ›› Issue (13): 365-339.doi: 10.7506/spkx1002-6630-20241224-191

• 安全检测 • 上一篇    

QuEChERS法同时测定水产品中邻苯二甲酸酯及其代谢物的含量

林伟健,张艺严,黄育坊,王姣姣,李敏倩,吕辉雄,黄晓梅   

  1. (1.华南农业大学资源环境学院,广东 广州 510642;2.广东省农业科学院农业质量标准与监测技术研究所,广东 广州 510640;3.华南农业大学海洋学院,广东 广州 510642;4.广东省农产品质量安全风险评估重点实验室,广东 广州 510640;5.猪禽种业全国重点实验室,广东 广州 510640)
  • 发布日期:2025-06-13
  • 基金资助:
    广东省基础与应用基础研究基金项目(2024A1515030031;2023A1515012091); 广州市基础与应用基础项目(2023A04J0785;2023A04J0782); 广东省农业科学院猪禽种业全国重点实验室2023年度自主科研项目(2023QZ-NK15)

QuEChERS Method for Simultaneous Determination of Phthalates and Their Metabolites in Aquatic Products

LIN Weijian, ZHANG Yiyan, HUANG Yufang, WANG Jiaojiao, LI Minqian, LÜ Huixiong, HUANG Xiaomei   

  1. (1. College of Natural Resources and Environment, South China Agricultural University, Guangzhou 510642, China; 2. Institute of Quality Standard and Monitoring Technology for Agro-products, Guangdong Academy of Agricultural Sciences, Guangzhou 510640, China; 3. College of Marine Sciences, South China Agricultural University, Guangzhou 510642, China; 4. Guangdong Provincial Key Laboratory of Quality & Safety Risk Assessment for Agro-products, Guangzhou 510640, China; 5. State Key Laboratory of Swine and Poultry Breeding Industry, Guangzhou 510640, China)
  • Published:2025-06-13

摘要: 基于QuEChERS法对水产品中19 种邻苯二甲酸酯(phthalate esters,PAEs)和9 种邻苯二甲酸单酯(phthalate monoesters,mPAEs)进行同时前处理后,采用超高效液相色谱-高分辨质谱法测定其PAEs和mPAEs的含量。结果显示,19 种PAEs和9 种mPAEs的基质加标平均回收率分别为71%~120%和87%~119%,方法检出限分别为1~48 ng/g(以干质量计,下同)和1~6 ng/g。值得注意的是,本研究通过优化色谱条件,实现了4 组PAEs和1 组mPAEs同分异构体的基线分离,尤其是邻苯二甲酸二丁酯(dibutyl phthalate,DBP)与邻苯二甲酸二异丁酯(diisobutyl phthalate,DIBP)、邻苯二甲酸单丁酯(monobutyl phthalate,MBP)与邻苯二甲酸单异丁酯(monoisobutyl phthalate,MIBP)。本方法应用于广州市17 种市售水产品,结果显示,水产品中DBP、DIBP、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸(4-甲基-2-戊基)酯、邻苯二甲酸丁苄酯、邻苯二甲酸二正戊酯6 种PAEs和MBP、MIBP、邻苯二甲酸单(2-乙基己基)酯3 种mPAEs的检出率较高。该方法操作简洁且灵敏度高,将为水产品中PAEs和mPAEs的检测和风险评估提供重要技术支撑。

关键词: 邻苯二甲酸酯;邻苯二甲酸单酯;超高效液相色谱-高分辨质谱法;水产品

Abstract: This study developed a method for the simultaneous determination of 19 phthalate esters (PAEs) and 9 phthalate monoesters (mPAEs) in aquatic products using ultra-high performance liquid chromatography-high-resolution mass spectrometry (UPLC-HRMS) after quick, easy, cheap, efficient, rugged and safe (QuEChERS) pretreatment. The results indicated that the average recoveries for 19 PAEs and 9 mPAEs in spiked matrices were 71%–120% and 87%–119%, with detection limits of 1–48 and 1–6 ng/g md, respectively. It was noted that under optimized chromatographic conditions, baseline separation of the isomers of four PAEs and one mPAE was achieved, especially diisobutyl phthalate (DIBP) versus dibutyl phthalate (DBP), and monoisobutyl phthalate (MIBP) versus monobutyl phthalate (MBP). This method was applied to 17 commercially available aquatic products in Guangzhou, and the results showed that the detection rates of six PAEs, including DBP, DIBP, di(2-ethylhexyl) phthalate, bis(4-methyl-2-pentyl) phthalate, butyl benzyl phthalate, di-n-pentyl phthalate, as well as three mPAEs, including MBP, MIBP, and mono(2-ethylhexyl) phthalate, were relatively high. This method is simple to operate, with high sensitivity, providing important technical support for the detection and risk assessment of PAEs and mPAEs in aquatic products.

Key words: phthalate esters; phthalate monoester; ultra-high performance liquid chromatography-high-resolution mass spectrometry; aquatic products

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