为了准确测定家兔血浆中的烟草特有N-亚硝胺(TSNAs),制备了四氮杂杯[2]芳烃[2]三嗪键合硅胶(NCS)固相萃取柱,并通过对NCS固相萃取、色谱及质谱条件的优化,建立了测定家兔血浆中的N-亚硝基降烟碱(NNN)、4-(N-甲基亚硝胺基)-1-(3-吡啶基)-1-丁酮(NNK)、4-(N-甲基亚硝胺基)-1-(3-吡啶基)-1-丁醇(NNAL)、N-亚硝基新烟草碱(NAT)和N-亚硝基假木贼碱(NAB)5种TSNAs的NCS固相萃取/HPLc.MS/MS方法。结果表明:NCS固相萃取柱对家兔血浆中5种TSNAs的萃取效率优于商品化的C18固相萃取柱;5种TSNAs的检测限为0.0092~0.0590ng/mL,回收率和相对标准偏差(RSD)分别为90.1%~113.3%和0.95%~7.22%。该方法简单、准确,适合于家兔血浆中TSNAs的检测。
In order to accurately determine the tobacco-specific N-nitrosamines ( TSNAs ), 4- ( methylnitrosa- mino) - 1-(3-pyridyl) - 1-butanone (NNK), 4-(methylnitrosamino)- 1-(3-pyridyl)- 1- butanol (NNAL), N-nitrosonor- nicotine (NNN), N-nitrosoanatabine (NAT) and N-nitrosoanabasine (NAB), in rabbit plasma, a solid-phase extrac- tion column using tetraazacalix[2]arene[2]triazine modified silica (NCS) as sorbent was prepared. A solid-phase extraction/HPLC-MS/MS method was established by optimizing NCS solid-phase extraction conditions, chro- matographic and mass spectrometric conditions. The results showed that NCS solid-phase extraction column was better than commercially available C18 solid-phase extraction column in terms of the extraction efficiency of 5 TSNAs. The limits of detection were 0.0092-0.0590 ng/mL, and the mean recoveries for each analyte ranged from 90.1% to 113.3% with the relative standard deviation (RSD) of 0.95%-7.22%. This method is simple, accu- rate and suitable for the determination of TSNAs in rabbit plasma.