Cooper S F, Lemoyne C, Gauvreau D
J Anal Toxicol. 1987 Jan-Feb;11(1):12-8. doi: 10.1093/jat/11.1.12.
A gas-liquid chromatographic method for quantitative determination of six volatile N-nitrosamines in human postmortem organs (brain, liver, kidneys, and pancreas) is described. This method, which is highly sensitive and selective, makes use of two different detectors, i.e., the electron capture detector (ECD) and the thermal energy analyzer (TEA). The mean absolute percentage recoveries of N-nitrosodimethylamine (NDMA), N-nitrosodiethylamine (NDEA), N-nitrosodipropylamine (NDPA), N-nitrosodibutylamine (NDBA), N-nitrosodipropylamine (NDPA, N-nitrosodibutylamine (NDBA), N-nitrosopiperidine (NPIP), and N-nitrosopyrrolidine (NPY) were 54.7, 80.0, 79.6, 72.5, 75.5, and 79.6, respectively. N-Nitrosamines in the organ extracts were converted to their corresponding N-nitramine analogs by pertrifluoroacetic acid oxidation. These derivatives were purified by adsorption chromatography on basic alumina and then analyzed by ECD. N-Nitrosamines were analyzed without derivatization in the organ extracts with the TEA detector. The described method did not cause artifactual formation of N-nitrosomethyl-N-butylamine (NMBA) when methyl-N-butylamine was used as an internal marker of nitrosation. NDMA was found in all the organs examined, whereas NDPA was only detected in the liver of one in four subjects. NDMA was found in all brain samples, indicating that it crosses the blood-brain barrier.
本文描述了一种采用气-液色谱法对人体死后器官（脑、肝、肾和胰腺）中的六种挥发性N-亚硝胺进行定量测定的方法。该方法具有高灵敏度和高选择性，采用了两种不同的检测器，即电子捕获检测器（ECD）和热能分析仪（TEA）。N-亚硝基二甲胺（NDMA）、N-亚硝基二乙胺（NDEA）、N-亚硝基二丙胺（NDPA）、N-亚硝基二丁胺（NDBA）、N-亚硝基哌啶（NPIP）和N-亚硝基吡咯烷（NPY）的平均绝对回收率分别为54.7%、80.0%、79.6%、72.5%、75.5%和79.6%。器官提取物中的N-亚硝胺通过全三氟乙酸氧化转化为相应的N-硝胺类似物。这些衍生物通过在碱性氧化铝上的吸附色谱法进行纯化，然后用ECD进行分析。N-亚硝胺在器官提取物中不经过衍生化，采用TEA检测器进行分析。当使用甲基-N-丁胺作为亚硝化的内标时，所描述的方法不会导致N-亚硝基甲基-N-丁胺（NMBA）的人为形成。在所检查的所有器官中均发现了NDMA，而NDPA仅在四分之一受试者的肝脏中检测到。在所有脑样本中均发现了NDMA，这表明它能够穿过血脑屏障。
