| This thesis has explored the application of using liquid chromatography - tandem mass spectrometry (LC-MS) as the major analytical tool in determining the trace amount of organic chemicals in food and in human plasma, and carefully tested the best operation conditions for measuring a range of individual trace level chemicals, and also discussed the optimization and mechanism of LC-MS parameter. In general, the following technical achievements could be concluded:1. A sensitive and selective liquid chromatography-tandem mass spectrometric (LC-MS) method has been developed to determine trace para red,Sudan I～IV,Sudan red B,Sudan red G,Sudan red 7B,Sudan Black B,Methyl Yellow,Toluidine Red,Fast Garnet GBC Base,Auramine,Oil Orange SS and Sudan Orange G in food, respectively. Samples were extracted using acetonitrile, then separated on a Agilent C18 column. Under the influence of organic acid in the mobile phase, MS detection using positive electrospray ionization as an interface is used in multiple reaction monitoring (MRM) mode to monitor transition. The limits of detection of dyes are attained at the level of ng·g-1. The established method has such advantage as high sensitivity,short analysis time,accurate quanlity,high recovery and good reproduce. It has provided a useful analytical method for the monitoring of the various Sudan dyes in food.2. A rapid and sensitive LC-MS method has been developed and validated for the identification and quantitation of rupatadine in human plasma after oral administration,zolmitriptan in human plasma after intranasal administration,the analysis of cetirizine in human plasma after oral intranasal administration and nalmefene in human plasma after intravenous infusion, respectively. Plasma samples were extracted using liquid-liquid extraction, then chromatographed on a column. Detection was performed on Agilent MSD Trap XCT ion-trap mass spectrometer connected to a Agilent 1100 high performance liquid chromatography (HPLC) by multiple reaction monitoring (MRM) mode or selected ion monitoring (SIM) mode via electrospray ionization (ESI) source or atmospheric pressure chemical ionization (APCI) source. The lower limit of quantitation (LOQ) can be identifiable and reproducible at 0.05μg· L-1. The proposed method is sensitive and reproducible enough to be used in pharmacokinetic, bioavailability or bioequivalence studies of these medicine.
|
PDF Full Text Request