Font Size: a A A

Application On Analysis Of Lipoid By LC/MS

Posted on:2010-08-19Degree:MasterType:Thesis
Country:ChinaCandidate:Y B JinFull Text:PDF
GTID:2180360305485982Subject:Drug Analysis
Abstract/Summary:PDF Full Text Request
As the developing of liquid chromatography-electrospray mass spectrometry, the mass spectrogram is becoming necessary and important in the medicine, chemistry, biology and sitiology. A highly sensitive LC/MS method was developed for the determination of lipoid.Lipoid is a kind of esters including phospholipids, glucolipids, lipoprotein and steroid, and so on. Gangliosides are a complex group of glycosphingolipids composed of oligoglycoceramides containing at least one sialic acid moiety. The ceramides are composed of sphingosine and fatty acids which may vary with respect to chain lengths and saturation. We developed a sensitive and rapid liquid chromatography-tandem mass spectrometry method for the quantitative determination of ganglioside (glucolipids) in milk and powder. Milk powder samples were extracted with methanol/water/chloroform and purified with a C18 SPE cartridge. Samples were then separated using a C4 column with the mobile phase of ammonium acetate-methanol in gradient elution. ESI-MS with the SIR monitoring was also used to detect and quantify the gangliosides included GM1, GM2, GM3, GD2 and GD3. The ganglioside GM1 was used as control standard, and GM1-d3 (m/z 1548) as internal standard. The peak areas ratios (Y) of sample TIC and internal standard were used for calculation the total count of gangliosides. The result showed the lower limit of quantitation of ganglioside was 0.500 ng-mL-1, and the linear range was 0.500-50.0 ng·mL-1. The inter-and intra-run precision (RSD) was less than 5%, and the recovery rate was 94%~114%. This method is proved to be specific, sensitive and accurate, which can be applied to determine the concentration of gangliosides in milk and powder. Lipoid Metabonomics focus on the changes of lipids,lipid metabolites and the factors interacting with lipid moleculars when organism is stressed by outer stimulation and interfered with diseases based on high-throughput detection and data analysis. Metabonomics based on LCMS is to detect the changes of lipoid molecular in simvastatin treated mouse serum which will provide useful methods in the mechanism of medicine and medicine safety assessment. The small molecular metabolites of mice serum were detected through metabonomics. The serum samples were analyzed by using UPLC/Q-TOF-MS and small molecules metabolite profiles from serum were obtained. Compared to control group, the intensity of Lyso-PC(16:0)、Lyso-PE(18:0)、Lyso-PE(20:1)、Cer(18:0/14:0)、Lyso-PC(14:0/14:0、Lyso-PC(14:1/14:1) was found to be changed. Through metabonomics, small molecular metabolites detected in serum were proved to be related to organism status by the addition of simvastatin. Metabonomics can be recognized as a technique for applications in pharmacy.The urine small molecular metabolites of mice were detected through metabonomics. The urine samples were analyzed by using UPLC/Q-TOF-MS and small molecules metabolite profiles from urine were obtained. Compared to control group, the intensity of palmitic acid, cholestane-pentol, oxo-androstenrone-glucuronide, DG and Lyso-PC were changed. Through metabonomics, small molecular metabolites detected in urine were proved to be related to organism status. Metabonomics can be recognized as a technique in many fields, such as mechanism of drug action, drug toxicity screening, clinical safety and disease diagnosis.
Keywords/Search Tags:LC/MS, Lipoid, Gangliosides, Content determination, Simvastatin, Metabonomics
PDF Full Text Request
Related items