Study On Capillary Electrophoresis And Related Techniques As Well As Applications In The Analysis Of Illicit Durgs

Due to high separation efficiency, low sample consumption and short analysistime, capillary electrophoresis (CE) has been paid more and more attentions since itwas first introduced by Jorgenson and Lukacs in1981. However, the development ofCE was limited in traditional detection methods (e.g. UV) with low detectionsensitivity results from the short optical path length within the detection cell. CEcoupled with mass spectrometry (MS), especially tandem mass spectrometry(MS/MS), has been proved as an ideal detection technique with excellent detectionsensitivity and the possibility of providing molecular and structural information forthe biological analysis. On line concentration technique is another simple method toimprove detection method without changing detector. Therefore, in this thesis,microemulsion electrokinetic chromatography (MEEKC) coupled with onlineconcentration technique, capillary electrophoresis-electrospray ionization massspectrometry (CE-ESI-MS) as well as CE-ESI-MS combined with onlineconcentration were studied and applied to separation and determination of illicit drugs.The thesis consists of the following four chapters.The first part is chapter1. In this chapter, the general introduction of MEEKC,CE-ESI-MS, techniques on the online concentration, the methods for the analysis ofillicit drugs as well as the purpose and signification of this thesis were described indetail.In chapter2, a rapid, sensitive and reproducible method using MEEKCcombined field amplified sample injection (FASI) for the analysis of nine narcoticswas developed. The simultaneous separation took place in about15min with LODsranging from0.3to8.0ng/mL (S/N=3) as well as satisfactory recoveries(79.4-119.9%). And the method has been successfully applied to the analysis of invitro metabolites of methadone.In chapter3, a simple method for rapid separation and sensitive detection ofstimulants and narcotics as well as their in vitro metabolites by online CE-ESI-MSwas established. In optimized conditions, the stimulants and narcotics were well separated within4.6min and the detection limits of the CE-ESI-MS analysis were inthe range of0.4-1.0ng/mL (S/N=3). The recoveries of spiked urine samples werebetween84.1%and108.0%with the RSDs lower than7.5%. The developed CE-MSmethod was also applied for the simultaneous analysis of methadone, pethidine andcodeine and their in vitro metabolites.In chapter4, an online CE-ESI-MS method was developed for the analysis ofanticholinergics. To improve the detection sensitivity of the method, FASI wasinvestigated in detail. Using field-amplified sample stacking, the detection limits werein the range of0.02-0.05ng/mL (S/N=3). Eventually, the proposed method has beensuccessfully applied for the analysis of anisodamine in real sample.