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×1.4μm)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1~200μg/L范围内线性关系良好,相关系数(r)为0.9996,相对标准偏差(RSD)为0.8%~6.0%,检出限为0.50μg/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1.29~3.75μg/kg,虾类样品检出值为0.50~2.63μg/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。
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-624 Sil MS(30 m×0.25 mm×1.4μm).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 1–200μg/L,with a good correlation coefficient(r2)of 0.9996,and the relative standard deviation(RSD)ranged 0.8–6.0%.The detection limit(3 S/N)was 0.50μg/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 1.29–3.75μg/kg for the fish samples and 0.50–2.63μg/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.
作者
陶森
孙金山
王雅玲
黄展锐
陈坤
谢凤慧
孙力军
励建荣
TAO Sen;SUN Jin-shan;WANG Ya-ling(Key Laboratory of Advanced Processing of Aquatic Products of Guangdong Higher Education Institution,Guangdong Provincial Key Laboratory of Aquatic Product Processing and Safety,College of Food Science and Technology,Guangdong Ocean University,Zhanjiang,Guangdong Province 524088,China;不详)
出处
《中国公共卫生》
CAS
CSCD
北大核心
2020年第10期1503-1506,共4页
Chinese Journal of Public Health
基金
国家自然科学基金(31871898)。
