食品科学 ›› 2025, Vol. 46 ›› Issue (19): 273-280.doi: 10.7506/spkx1002-6630-20250428-232

• 安全检测 • 上一篇    

固相萃取结合气相色谱-三重四极杆串联质谱法测定水产品中11 种苯并三唑类紫外吸收剂

雷承霖,龚艳,闻胜,周妍,曹文成,刘小方,陈海川,程青云,刘潇   

  1. (1.湖北省疾病预防控制中心,国家卫生健康委食品安全风险评估与标准研制特色实验室,湖北 武汉 430079;2.湖北工业大学生命科学与健康工程学院,湖北 武汉 430079;3.湖北省生物农药工程研究中心,湖北 武汉 430064)
  • 发布日期:2025-09-16
  • 基金资助:
    “十四五”国家重点研发计划重点专项(2023YFF1104800);湖北省自然科学基金项目(2022CFB022); 湖北省医学青年拔尖人才项目(S2020JY23)

Solid-Phase Extraction Combined with Gas Chromatography-Triple Quadrupole Tandem Mass Spectrometry for the Determination of 11 Benzotriazole Ultraviolet Stabilizers in Aquatic Products

LEI Chenglin, GONG Yan, WEN Sheng, ZHOU Yan, CAO Wencheng, LIU Xiaofang, CHEN Haichuan, CHENG Qingyun, LIU Xiao   

  1. (1. NHC Specialty Laboratory of Food Safety Risk Assessment and Standard Development, Hubei Provincial Centre for Disease Control and Prevention, Wuhan 430079, China; 2. School of Life and Health Sciences, Hubei University of Technology, Wuhan 430079, China; 3. Hubei Biopesticide Engineering Research Center, Wuhan 430064, China)
  • Published:2025-09-16

摘要: 采用固相萃取技术结合气相色谱-三重四极杆串联质谱仪,建立一种同时检测水产品中11 种苯并三唑类紫外吸收剂(benzotriazole ultraviolet stabilizers,BUVs)的方法。通过10 mL乙腈-水溶液(4∶1,V/V)超声提取后,加入2.5 g氯化钠盐析分层,上清液经3 次冷冻除脂后依次通过PRiME HLB和Florisil固相萃取柱净化浓缩。目标化合物使用DB-5MS色谱柱(30 m×0.25 mm,0.25 μm)进行分离,并在串联质谱的多反应监测(multiple reaction monitoring,MRM)模式下检测,同位素内标法定量。结果显示:11 种BUVs线性关系良好(R2>0.998),检出限为0.11~1.08 ng/g(以干质量计),定量限为0.33~3.24 ng/g(以干质量计)。在2、10、50 ng/g 3 个不同含量水平下进行加标回收实验,11 种BUVs的回收率为71.98%~119.08%,相对标准偏差小于19.60%。应用此方法对两类水产品进行检测,发现多种BUVs单体均有不同程度检出。该方法操作简单,重复性和精密度高,有效解决了高脂肪含量生物基质中BUVs的提取与净化问题,可为水产品中BUVs的准确定量分析提供有效技术支持。

关键词: 苯并三唑类紫外吸收剂;水产品;固相萃取;气相色谱-三重四极杆串联质谱法

Abstract: In this study, a method for the simultaneous determination of 11 benzotriazole ultraviolet stabilizers (BUVs) in aquatic products was developed using solid-phase extraction combined with gas chromatography-triple quadrupole tandem mass spectrometry. Samples were ultrasonically extracted with 10 mL of acetonitrile-water mixture (4:1, V/V), and added with 2.5 g of sodium chloride for salting out. The supernatant was concentrated after three rounds of freezing for degreasing, and then cleaned up by passing sequentially through PRiME HLB and Florisil solid-phase extraction (SPE) columns. The target compounds were separated using a DB-5MS (30 m × 0.25 mm, 0.25 μm) column, detected in the multiple reaction monitoring (MRM) mode by tandem mass spectrometry, and quantified by the isotope internal standard method. The results showed that good linearity (R2 > 0.998) was observed for the 11 BUVs, the limits of detection (LOD) ranged from 0.11 to 1.08 ng/g dry mass, and the limits of quantification (LOQ) ranged from 0.33 to 3.24 ng/g dry mass. At three different spiked concentrations, 2, 10, 50 ng/g, the recovery rates of these BUVs ranged from 71.98% to 119.08% with relative standard deviation (RSD) of less than 19.60%. In two types of aquatic products, a variety of BUV monomers at different concentrations were detected by the proposed method. This method is simple, reproducible and precise, and effectively solves the problem existing in the extraction and purification of BUVs from biological matrices with high fat content, providing effective technical support for the accurate quantitative analysis of BUVs in aquatic products.

Key words: benzotriazole ultraviolet stabilizers; aquatic products; solid phase extraction; gas chromatography-triple quadrupole tandem mass spectrometry

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