文献类型：期刊文献

中文题名：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

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

作者：陶森[1,2];孙金山[3];王雅玲[1];黄展锐[1];陈坤[3];谢凤慧[3];孙力军[1];励建荣[4]

机构：[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]阳江市检测检验中心;[3]深圳市通量检测科技有限公司;[4]渤海大学辽宁省食品安全重点实验室

年份：2020

卷号：36

期号：10

起止页码：1503

中文期刊名：中国公共卫生

外文期刊名：Chinese Journal of Public Health

收录：CSTPCD、、北大核心2017、CSCD2019_2020、北大核心、CSCD

基金：国家自然科学基金(31871898)。

语种：中文

中文关键词：水产干制品;QuEChERS;气相色谱-质谱(GC-MS);N–二甲基亚硝胺(NDMA)

外文关键词：dried aquatic products;QuEChERS;gas chromatography-mass spectrometry;N-dimethylnitrosamine

中文摘要：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。

外文摘要：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.