Ojala M, Poutanen M, Mattila I, Ketola R A, Kotiaho T, Kostiainen R
VTT Chemical Technology, P.O. Box 1403, 02044 VTT, Finland.
Rapid Commun Mass Spectrom. 2000;14(11):994-8. doi: 10.1002/(SICI)1097-0231(20000615)14:11<994::AID-RCM977>3.0.CO;2-6.
A method using purge-and-membrane mass spectrometry (PAM-MS) was developed for the analysis of residual solvents in pharmaceutical products. The method combines dynamic headspace and membrane inlet mass spectrometry. The limits of detection for the compounds studied, benzene, toluene, chloroform, 2-pentene and 2-methyl- and 3-methylpentane, were 0.05-0.1 mg/kg. In quantitative analysis the method showed good linearity (r(2) > 0.998) and acceptable within-day (RSD = 7.9-18%) and between-day (RSD = 6.8-10%) repeatability. The PAM-MS method combined with the custom-made Solver program was compared with a method using purge-and-trap gas chromatography/mass spectrometry (P&T-GC/MS) for identification of residual solvents from authentic samples. The results showed that PAM-MS/Solver provides reliable identification of the main volatile organic compounds (VOCs) in the pharmaceuticals, but VOCs with low concentrations (below 0.5 mg/kg) were better identified by P&T-GC/MS. Other advantages of the PAM-MS method were short analysis times and non-requirement for pre-treatment of samples.
开发了一种采用吹扫-膜质谱法（PAM-MS）分析药品中残留溶剂的方法。该方法结合了动态顶空和膜进样质谱技术。所研究化合物苯、甲苯、氯仿、2-戊烯以及2-甲基戊烷和3-甲基戊烷的检测限为0.05 - 0.1 mg/kg。在定量分析中，该方法显示出良好的线性（r(2) > 0.998）以及可接受的日内（RSD = 7.9 - 18%）和日间（RSD = 6.8 - 10%）重复性。将PAM-MS方法与定制的Solver程序相结合，与采用吹扫捕集气相色谱/质谱法（P&T-GC/MS）从真实样品中鉴定残留溶剂的方法进行了比较。结果表明，PAM-MS/Solver能可靠鉴定药品中的主要挥发性有机化合物（VOCs），但低浓度（低于0.5 mg/kg）的VOCs用P&T-GC/MS能更好地鉴定。PAM-MS方法的其他优点是分析时间短且无需对样品进行预处理。
