USP’s colleague Kosuri et al. published this week, “GC-MS/MS method for trace level quantification of six nitrosamines impurities (NDMA, NDEA, NEIPA, NDIPA, NDPA, and NDBA) in commercially used organic solvents: Dichloromethane, Ethyl acetate, Toluene, and o-Xylene” in the Journal of Pharmaceutical Sciences.
The quantification of nitrosamines in commercial-grade solvents ranged from 100 ppb to 8000 ppb with respect to the sample concentration of 25 mg/mL with good sensitivity in LOQ level. The quantification ranged from 5 ppb (for NDMA, NDEA, NEIPA, NDIPA, NDPA) and 13 ppb (NDBA) to 2000 ppb with respect to the sample concentration of 100 mg/mL for analytical grade solvents with good sensitivity in the proposed method.
Thanks for the article.
At the user level, say that the problem of solvents is not in commercial solvents. The analytical problem derives from the plant recovery of solvents from different processes. The analytical matrix becomes very complex and these simple approximation methods are insufficient. Nor do I see that they take into account the level of DMF that the samples contain and that they interfere with NDMA. There are also maskers… I’m sorry to say that the bar is on another level. We are being asked for more by the authorities.
At the industry level the only option is to go to high resolution gases.The criticism is that there are no methods that meet the expectations of the regulatory agent.