Hwang Joung Boon, Lee Jung Eun, Kim Eunbi, Eom Kwon Yong, Kim Hyun-Ah, Lee Soonho
National Institute of Food and Drug Safety Evaluation, Food Additives and Packaging Division, Cheongju, South Korea.
Korea Food and Drug Administration-Advanced Analysis Team, Cheongju, South Korea.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2023 Apr;40(4):518-527. doi: 10.1080/19440049.2023.2193276. Epub 2023 Mar 27.
A simple and sensitive method based on liquid chromatography-atmospheric pressure chemical ionisation-tandem mass spectrometry (LC-APCI-MS/MS) was developed and validated to determine the levels of 13N-nitrosamines and N-nitrosatable substances migrated from rubber teats into artificial saliva. The migration test from rubber teats was conducted at 40 °C and for 24 h in artificial saliva, and the migrated artificial saliva solution was analysed by liquid chromatography tandem mass spectrometry (LC-MS/MS) without further extracting steps. The sensitivity of N-nitrosamines was examined by applying atmospheric chemical ionisation and electrospray ionisation to optimise the mass spectrometric conditions, and the atmospheric chemical ionisation (APCI) mode exhibited 1.6-19 times higher sensitivity. Method validation showed acceptable linearity, precision, and accuracy, and the detection and quantification limits were 0.07-0.35 and 0.24-1.1 μg kg, respectively. The developed liquid chromatography-atmospheric chemical ionisation-tandem mass spectrometry method was applied to 39 domestic and imported rubber teats. From 39 samples, N-nitrosamines [N-nitrosodimethylamine (NDMA), N-nitrosomorpholine (NMOR), and N-nitroso n-methyl N-phenylamine (NMPhA)] were detected in 30 samples, with N-nitrosatable substances in 17 samples give rise to NDMA, NMOR, and N-nitrosodiethylamine. However, the levels were below the specific migration limit of Korean Standards and Specifications for Food Containers, Utensils, and Packages and EC Directive 93/11/EEC.
建立并验证了一种基于液相色谱 - 大气压化学电离 - 串联质谱法(LC - APCI - MS/MS)的简单灵敏方法,用于测定从橡胶奶嘴迁移到人工唾液中的13种N - 亚硝胺和N - 亚硝化物质的含量。在40°C下于人工唾液中对橡胶奶嘴进行24小时的迁移试验,迁移后的人工唾液溶液不经进一步提取步骤,直接用液相色谱串联质谱法(LC - MS/MS)进行分析。通过应用大气压化学电离和电喷雾电离来优化质谱条件,考察了N - 亚硝胺的灵敏度,结果表明大气压化学电离(APCI)模式的灵敏度高1.6 - 19倍。方法验证显示该方法具有可接受的线性、精密度和准确度,检测限和定量限分别为0.07 - 0.35 μg/kg和0.24 - 1.1 μg/kg。所建立的液相色谱 - 大气压化学电离 - 串联质谱法应用于39个国产和进口橡胶奶嘴。在39个样品中,30个样品检测出N - 亚硝胺[N - 亚硝基二甲胺(NDMA)、N - 亚硝基吗啉(NMOR)和N - 亚硝基 - N - 甲基 - N - 苯胺(NMPhA)],17个样品中的N - 亚硝化物质产生了NDMA、NMOR和N - 亚硝基二乙胺。然而,这些含量低于韩国食品容器、器具和包装的标准与规范以及欧盟委员会指令93/11/EEC的特定迁移限量。