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陶森, 孙金山, 王雅玲, 黄展锐, 陈坤, 谢凤慧, 孙力军, 励建荣. 水产干制品中N–二甲基亚硝胺QuEChERS低温萃取及GC-MS检测方法建立[J]. 中国公共卫生, 2020, 36(10): 1503-1506. DOI: 10.11847/zgggws1121517
引用本文: 陶森, 孙金山, 王雅玲, 黄展锐, 陈坤, 谢凤慧, 孙力军, 励建荣. 水产干制品中N–二甲基亚硝胺QuEChERS低温萃取及GC-MS检测方法建立[J]. 中国公共卫生, 2020, 36(10): 1503-1506. DOI: 10.11847/zgggws1121517
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TAO Sen, SUN Jin-shan, WANG Ya-ling, . Detection of N-dimethylnitrosamine in dried aquatic products with QuEChERS low temperature extraction and GC-MS[J]. Chinese Journal of Public Health, 2020, 36(10): 1503-1506. DOI: 10.11847/zgggws1121517
Citation: TAO Sen, SUN Jin-shan, WANG Ya-ling, . Detection of N-dimethylnitrosamine in dried aquatic products with QuEChERS low temperature extraction and GC-MS[J]. Chinese Journal of Public Health, 2020, 36(10): 1503-1506. DOI: 10.11847/zgggws1121517
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水产干制品中N–二甲基亚硝胺QuEChERS低温萃取及GC-MS检测方法建立

Detection of N-dimethylnitrosamine in dried aquatic products with QuEChERS low temperature extraction and GC-MS

    摘要
  • 摘要:
      目的  采用改进的QuEChERS法辅以低温条件进行提取和净化，建立气相色谱－质谱（GC-MS）/SIM方法，快速测定水产干制品中N – 二甲基亚硝胺含量。
      方法  称样5 g，经乙酸乙酯（10 mL）提取，冷冻离心，提取液经十八烷基硅烷键合硅胶（C18）和乙二胺 – N – 丙基硅烷（PSA）净化，采用 Rxi-624 Sil MS毛细管色谱柱（30 m × 0.25 mm × 1.4 μm）分离，选择离子监测（SIM）模式进行测定，外标法定量。
      结果  N – 二甲基亚硝胺在1～200 μg/L范围内线性关系良好，相关系数（r）为0.999 6，相对标准偏差（RSD）为0.8 %～6.0 %，检出限为0.50 μg/kg，加标回收率为88.0 %～101.6 %。对湛江市东风水产批发市场采集的鱼、虾、贝类样品检测结果显示，鱼类和虾类样品中均有N – 二甲基亚硝胺检出，贝类样品中未检出。鱼类样品检出量为1.29～3.75 μg/kg，虾类样品检出值为0.50～2.63 μg/kg。
      结论  该法简便快速，灵敏有效，适用于水产干制品中N – 二甲基亚硝胺含量的快速筛查和测定。

     

    Abstract:
      Objective  To establish a modified quick, easy, cheap, effective, rugged, safe (QuEChERS) method for rapid detection of N-dimethylnitrosamine (NDMA) in dried aquatic products with gas chromatography-mass spectrometry/selected ion monitoring (GC-MS/SIM) and low temperature extraction and purification.
      Methods  Five grams of sample was extracted with ethyl acetate (10 mL) and centrifuged under refrigeration; the extract was purified by octadecylsilane-bonded silica gel (C18) and ethylenediamine-N-propylsilane (PSA) and separated using capillary column Rxi-624Sil MS (30 m × 0.25 mm × 1.4 μm). NDMA in the samples was detected with SIM and quantified by external standard method.
      Results  The calibration curve of NDMA was linear in the range of 1 – 200 μg/L, with a good correlation coefficient (r2) of 0.999 6, and the relative standard deviation (RSD) ranged 0.8 – 6.0%. The detection limit (3 S/N) was 0.50 μg/kg. The recovery of standard addition was between 88% – 102%. The NDMA was detected in fish and shrimp samples but not in shellfish samples collected in a aquatic product market in Zhanjiang city; the detected NDMA contents were 1.29 – 3.75 μg/kg for the fish samples and 0.50 – 2.63 μg/kg for the shrimp samples.
      Conclusion  The established method is simple, rapid, sensitive and effective, and is suitable for rapid screening and determination of N-dimethylnitrosamine content in dried aquatic products.

     

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