LC-MS/MS法测定口含烟中的4种亚硝基氨基酸

Determination of four N-nitrosamino acids in oral smokeless tobacco products by LC-MS/MS

建立了液相色谱-四级杆串接质谱(LC-MS/MS)测定口含烟中N-亚硝基肌氨酸(NSAR)、3-(N-甲基亚硝基氨基)丙酸(MNPA)、4-(N-甲基亚硝基氨基)丁酸(MNBA)、亚硝基氮杂环丁烷-2-羧酸(NAzCA)的分析方法。样品经水萃取,硅藻土液液萃取柱净化后浓缩,进LC-MS-MS分析。结果表明:①NSAR、NAzCA、MNPA、MNBA的检出限分别为5.0 ng/g、2.4 ng/g、5.7 ng/g、1.4 ng/g,日内精密度小于6.5%,日间精密度小于9.4%,回收率在77.7%~111%之间。②分析了国内外14种口含烟,胶基型和含化型制品未检出4种亚硝基氨基酸;口含型样品中部分检出NSAR、NAzCA,均检出MNPA及MNBA,含量范围分别为ND~128.3 ng/g、ND~141.6 ng/g、1687.1~2424.1 ng/g、65.0~199.5 ng/g。该方法简单、准确,适用于口含烟中4种亚硝基氨基酸的分析。

A liquid chromatography-electrospray ionization tandem mass spectrometric(LC-MS/MS)method has been developed for the determination of N-Nitrososarcosine(NSAR)、3-(N-methylnitrosamino)propionic acid(MNPA)、4-(N-methylnitrosamino)butyric acid(MNBA)、Nitrosoazetidine-4-carboxylic acid(NAzCA)in oral smokeless tobacco products.The samples were extracted by water,purified by liquid-liquid diatomite extraction column and concentrated,and then analyzed by LC-MS-MS.The experimental results revealed:1)The detection limits of NSAR、NAzCA、MNPA、MNBA were 5.0 ng/g、2.4 ng/g、5.7 ng/g、1.4 ng/g respectively,the within-day and inter-day precisions were less than 6.5%and 9.4%,the recoveries ranged from 77.7%to 111%.2)14 oral smokeless tobacco products were analyzed,the four N-nitrosamino acids were not detected in nicotine chewing gums and dissolvable tobacco products,NSAR and NAzCA were partially well MNPA and MNBA were entirely detected in snus and moist snuff with contents ranging from ND~128.3 ng/g、ND~141.6 ng/g、1687.1~2424.1ng/g、65.0~199.5 ng/g respectively.The method is simple,accurate and suitable for the analysis of four N-nitrosamino acids in oral smokeless tobacco products.