目的 建立GC-MS/MS法測(cè)定甲磺酸卡莫司他原料藥中的亞硝胺類基因毒性雜質(zhì)N-亞硝基二甲胺（NDMA）。方法 采用Agilent DB-SELECT 624UI色譜柱（30 m×0.32 mm×1.80 μm）色譜柱，離子源為EI源，采用多反應(yīng)監(jiān)測(cè)模式，以m/z74→44.2為定量離子，m/z 74→42.2為定性離子，進(jìn)行數(shù)據(jù)采集。結(jié)果NDMA在12.571 2～100.569 6 ng/mL線性良好（r=0.997 6），檢測(cè)限質(zhì)量濃度為5.028 5 ng/mL，平均回收率為107.4%，RSD值為2.5%。結(jié)論 該方法操作簡(jiǎn)單，靈敏度高，專屬性和重復(fù)性好，可用于甲磺酸卡莫司他原料藥中NDMA的檢測(cè)。

Objective To establish a GC-MS/MS method for determination of genotoxic impurityN-nitrosodimethylamine (NDMA) in camostat mesylate active pharmaceutical ingredients.Methods NDMA was determined by GC-MS/MS method with Agilent DB-SELECT 624UI column (30 m×0.32 mm×1.8 μm). The mass spectrometer was operated in the electron impact ionization (EI) fixed mode, and the ion collection mode was multiple reaction monitoring (MRM). The ion for quantitative wasm/z74 → 44.2, and for qualitative wasm/z 74 → 42.2.Results NDMA had a good linear relationship 12.571 2 — 100.569 6 ng/mL withr = 0.997 6. The limit of detection (LOD) was 5.028 5 ng/mL. The average recovery was 107.4%with RSD value 2.5 %.Conclusion The method is convenient sensitive, specific, and reproducible, which is suitable for determination of NDMA in camostat mesylate active pharmaceutical ingredients.

R927.2