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13C 및 15N 안정성 동위원소 비율 분석에 의한 원료의약품에서 에페드린 및 슈도에페드린의 기원 판별
백승경(SeungKyung Baeck),Tetsuo Nagano,최화경(HwaKyung Choi),정희선(HeeSun Chung),표명윤(MyungYun Pyo),정진일(JinIl Jeong),양원경(Wonkyang Yang),Yukiko Makino,장문희(MoonHee Jang) 대한약학회 2009 약학회지 Vol.53 No.5
The abuse of methamphetamine (MA) is one of the most serious drug abuses in Asia. And, the prevention of precursor production for abuse drug is one of the most effective drug control system. Isotope ratio analysis at natural abundance levels have been used to establish the environmental source or the geographic origin of various biological and nonbiological materials. Ephedrine, the precursor of MA, is produced by one of three methods; extraction from Ephedra plants, full chemical synthesis or via a semi-synthetic process involving the fermentation of sugar, followed by amination. We investigated the origin of ephedrine and pseudoephedrine based on the carbon and nitrogen values for nineteen pharmaceutical powder materials (PPMs) obtained from pharmaceutical company in Korea by stable isotope ratio mass spectrometry coupled to an elemental analyser (EA-IRMS). The carbon delta values for the ephedrine and pseudoephedrine were -24.21~-22.72 (mean=-23.72) ‰ and -23.79~-22.71 (mean=-23.48) ‰. The nitrogen delta values were 3.51~5.55 (4.43) ‰ and 2.24~8.22 (5.42) ‰. These results indicate that PPMs are semi-synthetic products. Therefore the origins of ephedrine (natural, semi-synthetic or synthetic) could be discriminated by using carbon and nitrogen stable isotope ratios. we are sure tat this stable isotope ratio analysis can discriminate the origins of precursors of methamphetamine.
타액 중 Δ9-Tetrahydrocannabinol 및 11-Nor-9-carboxy-Δ9-Tetrahydrocannabinol의 분석법 확립 및 안정성 검토
최혜영(Hyeyoung Choi),백승경(Seungkyung Baeck),장문희(Moonhee Jang),최화경(Hwakyung Choi),정희선(Heesun Chung) 대한약학회 2010 약학회지 Vol.54 No.4
Oral fluid has become increasingly popular as an alternative specimen in the field of driving under the influence of drugs (DUID) and work place drug testing. In this study, an analytical method for the detection and quantification of Δ9-tetrahydrocannabinol (THC) and its metabolite, 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THC-COOH) in oral fluid by SPE and GC-MS was established and fully validated. The stability of THC and THC-COOH in oral fluid during storage was also determined by examining the THC and THC-COOH concentration changes depending on time and container materials. Oral fluid samples were kept over 21 days at room temperature, -4oC and -20oC in two different specimen collection tubes; glass and polypropylene tubes. Three replicates for each condition with different temperature and types of a container were analyzed at five different time points over 21 days. When oral fluid samples were stored in glass tubes, the loss of both THC and THC-COOH was less than 10% at all room temperature, -4oC and -20oC. However, in polypropylene tubes, the loss of both THC and THC-COOH increased significantly over the study period. In particular, the concentration of THC decreased more rapidly than that of THC-COOH at room temperature and the maximal percentage of THC lost was 90.3% after 21 days. The result indicates that it would be necessary to collect oral fluid samples in glass containers and cool the samples until analysis in order to prevent the degradation of analytes.
Lee, Sooyeun,Kang, So-young,Ji, Dajeong,Baeck, Seungkyung,Lee, Sangki,Oh, Seung Min,Chung, Kyu Hyuck Springer-Verlag 2013 Analytical and bioanalytical chemistry Vol.405 No.10
<P>The chemical castration law, which targets child molesters with recidivism, was introduced in Korea in 2011. For this, leuprolide, a gonadotropin-releasing hormone agonist, is used to decrease testosterone production and suppress libido. In order to achieve efficient law enforcement, it is necessary to monitor intentional ingestion of drugs that antagonize the effect of leuprolide. Therefore, an analytical method for the simultaneous detection of mirodenafil, sildenafil, tadalafil, udenafil, vardenafil, icariin, alprostadil, and yohimbine, which are the major impotence treatment drugs, legitimately or otherwise, in Korea, as well as their selected metabolites, in human urine was established and validated using liquid chromatography-tandem mass spectrometry (LC-MS/MS). First, different sample preparation methods, two solid-phase extractions with different cartridges and protein precipitation, were compared and protein precipitation was chosen for the entire study because it showed better matrix effects and recoveries. Thus, the drugs and metabolites in urine were extracted by protein precipitation and then filtered and analyzed by LC-MS/MS with polarity switching electrospray ionization. The validation results of selectivity, matrix effect, recovery, linearity, intra- and inter-assay precision and accuracy were satisfactory. The limits of detection ranged from 0.25 to 10 ng/mL, and the limits of quantification were 2.5 to 50 ng/mL. The drugs and metabolites in urine did not show any degradation under storage for 7 and 15 days at 4 and -20 C as well as after three freeze-thaw cycles. The developed method will be very useful for monitoring the illegal use of impotence treatment drugs.</P>