食品科学 ›› 2016, Vol. 37 ›› Issue (24): 164-169.doi: 10.7506/spkx1002-6630-201624025

• 安全检测 • 上一篇    下一篇

高效液相色谱-串联质谱法测定3种水产品中的T-2毒素与HT-2毒素

王小博,施 琦,王雅玲,廖建萌,刘 阳,吴移山,高 平,励建荣   

  1. 1.广东海洋大学食品科技学院,广东省水产品加工与安全重点实验室,广东普通高等学校水产品深加工重点实验室,广东 湛江 524088;2.广东省湛江市质量计量监督检测所,国家海产品质量监督检验中心(湛江),广东 湛江 524096; 3.湛江市食品药品监督管理局,广东 湛江 524022;4.渤海大学 辽宁省食品安全重点实验室,辽宁 锦州 121013
  • 出版日期:2016-12-25 发布日期:2016-12-21
  • 基金资助:
    国家自然科学基金面上项目(31171634;31371777);广东省科技计划项目(2014B020205006);广东省海洋与渔业局项目(粤财农[2015]115号)

Determination of T-2 and HT-2 Toxins in Three Aquatic Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

WANG Xiaobo, SHI Qi, WANG Yaling, LIAO Jianmeng, LIU Yang, WU Yishan, GAO Ping, LI Jianrong   

  1. 1. Guangdong Provincial Key Laboratory of Aquatic Product Processing and Safety, Key Laboratory of Advanced Processing of Aquatic Products of Guangdong Higher Education Institution, College of Food Science and Technology, Guangdong Ocean University, Zhanjiang 524088, China; 2. Zhanjiang Institute of Supervision & Test on Quality & Measure, National Marine Products Quality Supervision & Inspection Center, Zhanjiang 524096, China; 3. Zhanjiang Food and Drug Administration, Zhanjiang 524022, China; 4. Liaoning Key Laboratory of Food Safety, Bohai University, Jinzhou 121013, China
  • Online:2016-12-25 Published:2016-12-21

摘要: 建立高效液相色谱-串联质谱定量快速检测罗非鱼、南美白对虾和黄金贝中的T-2毒素与HT-2毒素方法。以10 mL乙酸乙酯作为提取溶剂,振荡提取,无水硫酸钠除水,定量移取5 mL提取液氮气吹干后用1 mL含有0.1%甲酸的甲醇-5 mmol/L乙酸铵溶液(3∶7,V/V)复溶,正己烷脱脂净化,基质匹配法外标定量。3 种水产品中T-2毒素和HT-2毒素的检出限分别为2 μg/kg和4 μg/kg。T-2毒素质量浓度为2~100 ng/mL,HT-2毒素质量浓度为4~200 ng/mL,范围内线性良好。在3 种样本中进行3 个水平添加实验(n=6),T-2毒素回收率为84.3%~109.9%,HT-2毒素的回收率为90.9%~103.2%。T-2毒素的相对标准偏差为2.0%~8.7%,HT-2毒素的相对标准偏差为2.6%~10.6%。本方法简便快速、准确度好、精密度高,适用于3 种代表性水产品中T-2与HT-2毒素的同时检测。

关键词: T-2毒素, HT-2毒素, 高效液相色谱-串联质谱

Abstract: A fast high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the quantitative determination of T-2 and HT-2 toxins in tilapia, Litopenaeus vannamei and golden scallop. After being homogenized, samples were extracted with 10 mL of neutral ethyl acetate by vibration, and after removing the moisture with sodium sulfate, 5 mL of the upper layer was concentrated with nitrogen blowing, re-dissolved with 1 mL of 0.1% formic acid in methyl alcohol:5 mmol/L ammonium acetate (3:7, V/V), and degreased with hexane. The target compounds were quantified by the matrix-matched external standard method. Under optimized conditions, the lower limits of quantitation (LLOQs) for T-2 and HT-2 toxins in three aquatic products were 2 and 4 μg/kg, respectively. The linear range was 2–100 ng/mL for T-2 toxin and 4–200 ng/mL for HT-2 toxin. The average recoveries for three aquatic samples at three spiked levels ranged from 84.3% to 109.9% for T-2 toxin and 90.9% to 103.2% for HT-2 toxin. The relative standard deviations (RSDs) were in a range of 2.0%–8.7% for T-2 toxin and 2.6%–10.6% for HT-2 toxin (n = 6). The method is simple, rapid, accurate, precise and suitable for the simultaneous detection of T-2 and HT-2 toxins in the three representative aquatic products.

Key words: T-2 toxin, HT-2 toxin, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)

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