After a presence of highly hepatotoxic and potentially carcinogenic N‐nitrosodimethylamine was detected in certain lots of sartan, ranitidine, metformin, and other pharmaceuticals, local regulatory authorities issued recalls of suspected products, and concerns of the pharmacotherapy safety were widely discussed. Since then, testing of a representative sample of each produced lot of these pharmaceuticals is required as a part of quality control processes. Hence, an interface‐free CE‐nanoESI system coupled with MS detection was employed for the development of a simple and economical method for quantitative detection of this contaminant in the valsartan drug substances and finished formulations used as model matrices. In this arrangement, a fused‐silica capillary was used as both a separation column and a nanoESI emitter providing high ionization efficiency and sensitivity. The optimized procedure was found to have sufficient selectivity, linearity, accuracy, and precision. The established LOD and LOQ values were 0.3 and 1.0 ng/mL, respectively. The practical applicability of the method was tested by analyses of commercially available Valsacor^® tablets. The results obtained prove that the developed procedure represents a promising alternative to currently available GC‐ and LC‐based methods. Furthermore, after an adjustment of the separation conditions, the CE‐nanoESI/MS system can be conceptually used for the determination of NDMA in other suspected pharmaceuticals.

中文翻译：

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毛细管电泳-纳米电喷雾电离-质谱法在药物中N-亚硝基二甲胺的测定中的应用

在存在高肝毒性和潜在致癌性的N 后部分批次沙坦类、雷尼替丁、二甲双胍等药品中检出-亚硝基二甲胺，当地监管部门发布疑似产品召回，对药物治疗安全性的担忧引起广泛讨论。从那时起，作为质量控制过程的一部分，需要对每批生产的这些药物的代表性样品进行测试。因此，采用无界面 CE-nanoESI 系统与 MS 检测相结合，开发了一种简单经济的方法，用于定量检测缬沙坦原料药和用作模型基质的成品制剂中的这种污染物。在这种布置中，熔融石英毛细管用作分离柱和 nanoESI 发射器，提供高电离效率和灵敏度。发现优化的程序具有足够的选择性、线性、准确度和精密度。确定的 LOD 和 LOQ 值分别为 0.3 和 1.0 ng/mL。通过对市售 Valsacor 的分析测试了该方法的实际适用性^®片。获得的结果证明，所开发的程序代表了当前可用的基于 GC 和 LC 的方法的有前途的替代方法。此外，在调整分离条件后，CE-nanoESI/MS 系统在概念上可用于测定其他可疑药物中的 NDMA。