Titanium dioxide solid-phase dynamic extraction - gas chromatographic- mass spectrometry for dihydro-deoxycodeine opiate analysis

• Main Authors: Chi-Ju Su, 蘇紀如
• Other Authors: Hun-Chi Shu
• Format: Others
• Language: zh-TW
• Published: 2009
• Online Access: http://ndltd.ncl.edu.tw/handle/99903317080877926743

碩士 === 國立東華大學 === 化學系 === 97 === Dihydro-deoxycodeine opiate was synthesized by a new path with higher yield and purity. The titanium dioxide film in inside of the needle preparing by sol-gel method was applied as the solid-phase dynamic extraction (SPDE) with GC-MS to analysis dihydro-deoxycodeine opiate drugs. The optimize conditions of the method are that sol-gel stirring time is 30 min, coating one layer at pH 3. The adsorption time is setting 30 min without salt addition and the desorption time is 10 min at 290 ℃. Two type of the solid-phase dynamic extraction methods, SPDE-1 and SPDE-2 for internal standard (IS) addition were studied. In SPDE-1, IS was added in samples and then extracted by SPDE needle; on the other hand, SPDE-2 is that the IS was injected in GC-MS before the thermal desorption. In short, SPDE-2 is more sensitive and wider linear range then SPDE-1, and preventing that the Impurities influence deuterium IS in urine. For the SPDE method, the retention times of analyte and IS are the same (r.t.:34.21 min) and the regression coefficients (R2) of calibration curve showing the good liner correlation were varying from 0.9958 to 0.9999 and prominent sensitivity. The limit of quantization (LOQ) of SPDE method is 1 ~5 ng/mL. The inter-day urine sample tested of RSD value of SPDE-2 was 10 ~ 12%, which means an acceptable reproducibility.