National Research Nuclear University MEPhI , 115409, Kashirskoe shosse 31, Moscow, Russian Federation.
Anal Chem. 2013 Oct 1;85(19):9003-12. doi: 10.1021/ac401191k. Epub 2013 Sep 17.
Recently developed ion mobility mass spectrometer is described. The instrument is based on a drift tube ion mobility spectrometer and an orthogonal acceleration electrostatic sector time-of-flight mass analyzer. Data collection is performed using a specially developed fast ADC-based recorder that allows real-time data integration in an interval between 3 and 100 s. Primary tests were done with positive ion electrospray. The tests have shown obtaining 100 ion mobility resolving power and 2000 mass resolving power. Obtained for 2,6-di-tert-butylpyridine in electrosprayed liquid samples during 100 s analysis and full IMS/MS data collection mode were 4 nM relative limits of detection and a 1 pg absolute limit of detection (S/N=3). Characteristic ion mobility/mass distributions were recorded for selected antibiotics, including amoxicillin, ampicillin, lomefloxacin, and ofloxacin. At studied conditions, lomefloxacin forms only a protonated molecule-producing reduced ion mobility peak at 1.082 cm(2)/(V s). Both amoxicillin and ampicillin produce M + H, M + CH3OH + H, and M + CH3CN + H. Amoxicillin shows two peaks at 0.909 cm(2)/(V s) and 0.905 cm(2)/(V s). Ampicillin shows one peak at 0.945 cm(2)/(V s). Intensity of protonated methanol containing cluster for both ampicillin and amoxicillin has a clear tendency to rise with sample keeping time. Ofloxacin produces two peaks in the ion mobility distribution. A lower ion mobility peak at 1.051 cm(2)/(V s) is shown to be formed by M + H ions. A higher ion mobility peak appearing for samples kept more than 48 h is shown to be formed by both M + H ion and a component identified as the M + 2H + M cluster. The cluster probably partly dissociates in the interface producing the M + H ion.
最近开发的离子淌度质谱仪得到了描述。该仪器基于漂移管离子淌度质谱仪和正交加速静电扇形飞行时间质谱分析仪。数据采集使用专门开发的基于快速 ADC 的记录器进行,该记录器允许在 3 到 100 秒的间隔内实时进行数据集成。初步测试是使用正离子电喷雾进行的。测试表明,该仪器获得了 100 的离子淌度分辨率和 2000 的质量分辨率。在 100 秒分析和全 IMS/MS 数据采集模式下,对电喷雾液体样品中的 2,6-二叔丁基吡啶进行测试,得到了 4 nM 的相对检出限和 1 pg 的绝对检出限(S/N=3)。记录了选定抗生素(包括阿莫西林、氨苄西林、洛美沙星和氧氟沙星)的特征性离子淌度/质量分布。在研究条件下,洛美沙星仅形成质子化分子,在 1.082 cm(2)/(V s)处产生降低的离子淌度峰。阿莫西林和氨苄西林都产生 M + H、M + CH3OH + H 和 M + CH3CN + H。阿莫西林在 0.909 cm(2)/(V s)和 0.905 cm(2)/(V s)处显示两个峰。氨苄西林在 0.945 cm(2)/(V s)处显示一个峰。对于阿莫西林和氨苄西林,含质子甲醇的加合离子强度都有随样品保存时间增加而明显上升的趋势。氧氟沙星在离子淌度分布中显示两个峰。在 1.051 cm(2)/(V s)处的较低离子淌度峰被证明是由 M + H离子形成的。对于保存时间超过 48 小时的样品,出现的较高离子淌度峰被证明是由 M + H离子和一个被鉴定为 M + 2H + M 加合离子的组分形成的。该加合离子可能在界面部分解离,产生 M + H离子。