气相色谱-质谱法测定质控样品鱼肉粉中N-亚硝基二甲胺含量

Determination of Contents of N-Nitrosodimethylamine in Fish Powder of Quality Control Sample by Gas Chromatography-Tandem Mass Spectrometry

目的:建立测定食品中N-亚硝基二甲胺(N-Nitrosodimethylamine, NDMA)含量的快速气相色谱串联质谱法。方法:利用气质联用法对质控样品鱼肉粉中NDMA进行检测,将GB 5009.26—2016中方法1的全玻璃蒸馏装置改成定氮仪单步蒸馏。结果:结果表明,在NDMA质量浓度范围为0.01-0.5μg/mL时,线性关系良好,相关系数R2=0.998,精密度实验计算相对标准偏差为4.6%,平均回收率为100.4%。该方法检出限为0.2μg/kg。结论:采用的蒸馏装置符合检测要求,具有密闭性好、效率高、蒸馏速度快等优点。可用于亚硝胺类化合物标准样品的质控考核,测定结果均在保证值范围内,准确度高。适用于食品中亚硝胺类化合物的检测。

Objective:To establish the determination of N-nitrosodimethylamine(NDMA)by gas chromatography-mass spectrometry.Methot:Gas chromatography-mass spectrometry and external standard method were used to determine NDMA in fish powder.Results:The results proved that when the concentration of NDMA ranges from 0.01μg/mL to 0.5μg/mL the linear relationship was good with a correlation coefficient of 0.998.The relative standard deviation was 4.6%,and the average recovery rate was 100.4%.The detection limit of method was 0.2μg/kg.Conclusion:The method can be applied to the quality control test of nitrosamines.The results were all within the guaranteed range with high accuracy.The method is suitable for the determination of nitrosamines in food.