Ranitidine drug products were recently recalled because they contained carcinogenic nitrosamines (NAs), such as N-nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA). This episode emphasises the importance of developing analytical methods to determine NAs in this type of product. This study describes the development and validation of an analytical method for the determination of nine NAs (NDMA, N-nitrosomethylethylamine (NEMA), NDEA, N-nitrosopyrrolidine (NPYR), N-nitrosomorpholine (NMOR) N-nitrosodi-n-propylamine (NDPA) N-nitrosopiperidine (NPIP), N-nitrosodi-n-butylamine (NDBA) and N-nitrosodiphenylamine (NDPhA)) in ranitidine drug samples using a combination of microextraction and gas chromatography-mass spectrometry. The procedure involved the dissolution of 1 g of sample in 10 mL of water. For the dispersive liquid-liquid microextraction, 0.5 g of NaCl was added to this aqueous solution, followed by a mixture containing 0.5 mL methanol as dispersant and 150 μL chloroform as extractant solvent. The recovered organic phase was injected into the GC-MS system and a 20 min oven programme was applied. Quantification limits were in the 0.21–21 ng g⁻¹ range, corresponding the lower limit to NDPhA and the higher to NDMA. Relative standard deviations lower than 12% were achieved in all cases, which indicates the adequate precision of the method. Seven pharmaceutical products containing two different amounts of ranitidine (150 and 300 mg) were analysed. None of the samples contained NEMA, NDEA, NPYR, NMOR, NDPA or NPIP, while NDMA, NDBA and NDPhA were found in three products.

雷尼替丁药物产品最近被召回，因为它们含有致癌的亚硝胺（NAs），例如N-亚硝基二甲胺（NDMA）和N-亚硝基二乙胺（NDEA）。这一集强调了开发分析方法以确定此类产品中NA的重要性。这项研究描述了测定九种NA（NDMA，N-亚硝基甲基乙胺（NEMA），NDEA，N-亚硝基吡咯烷（NPYR），N-亚硝基吗啉（NMOR）N-亚硝基二正丙基胺（NDMA）的分析方法的开发和验证雷尼替丁药物样品中的N-亚硝基哌啶（NPIP），N-亚硝基二正丁胺（NDBA）和N-亚硝基二苯胺（NDPhA））结合使用微萃取和气相色谱-质谱联用。该程序涉及将1 g样品溶解在10 mL水中。为了进行分散液-液微萃取，向该水溶液中加入0.5 g NaCl，然后加入含有0.5 mL甲醇作为分散剂和150μL氯仿作为萃取剂的混合物。将回收的有机相注入GC-MS系统，并应用20分钟的柱箱程序。定量限为0.21–21 ng g^-1范围，对应于NDPhA的下限，对应于NDMA的上限。在所有情况下，相对标准偏差均低于12％，这表明该方法具有足够的精度。分析了包含两种不同量雷尼替丁（150毫克和300毫克）的七个药品。样品均不含NEMA，NDEA，NPYR，NMOR，NDPA或NPIP，而在三种产品中均发现了NDMA，NDBA和NDPhA。