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도정아,이상경,노은영,윤순병,최호준,백선영,박성관 한국분석과학회 2017 분석과학 Vol.30 No.1
Anabolic steroids have similar structures to testosterone, both of which promote the growth of muscle mass and increase strength. However, the side effects of anabolic steroid use may lead to heart attacks or strokes. Additionally, the excessive use of steroids inhibits the production of the sex hormones in the body via a negative feedback loop, which results in testicular atrophy in males and amenorrhea in females. Currently, the method of choice used to test for the presence of anabolic steroids is GC-MS. However, GC-MS methods require chemical derivatization of the steroid sample to ensure compatibility with the analytical method; therefore, analysis of many different samples is difficult and time consuming. Unlike GC-MS, the liquid chromatography-quadrupoletime of flight mass spectrometry (LC-Q-TOF-MS) method is suitable for many samples. Twenty-two different anabolic steroids were analyzed by LC-Q-TOF-MS with various collision energies (CE). Accurate mass spectral data were obtained using a Q-TOF-MS equipped with an electro-spray ionization source and operated in the positive MS/MS mode for several classes of steroids that are often the targets of testing. Based on the collected data, fragmentation pathways were carefully elucidated. The high selectivity and sensitivity of the LC-Q-TOF-MS instrument combined with these fragmentation pathways offers a new approach for the rapid and accurate screening of anabolic steroids. The obtained data from the 22 different anabolic steroids will be shared with the scientific community in order to establish a library to aid in the screening of illegal anabolic steroids.
도정아,노은영,윤순병,박형준,조수열,박성관,윤창용 한국분석과학회 2015 분석과학 Vol.28 No.4
Phosphodiesterase type 5 inhibitors (PDE-5 inhibitors) are used in the treatment of erectile dysfunction. In recent years, a number of reports have been conducted on dietary supplements contaminated with PDE-5 analogues. In this study, 58 analogues of PDE-5 inhibitors were sorted into five groups: tadalafil, sildenafil, hongdenafil, vardenafil, and other analogues. These analogues were then evaluated using a liquid chromatographyquadrupole- time of flight mass spectrometry (LC-QTOF-MS) electrospray ionization mass method. Each compound has a unique fragmentation ion, which can be easily analyzed qualitatively. The fragmentation pathways of the analogues were elucidated based on the QTOF-MS and MS/MS data. Common ions were confirmed for each group by analyzing the structural characteristics and fragmentation pathways. Specifically, common ions were observed at m/z 169.08 and 135.04 (tadalafil analogues), m/z 311.15 and 283.12 (sildenafil analogues and hongdenafil analogues), and m/z 312.16 and 151.09 (vardenafil analogues). The advantage of this method is that the structure of unknown components can be determined by interpreting the product ions. Hence, the developed method can be used for the identification of unknown compounds. Fragmentation pathways may also aid in the detection and identification of PDE-5 inhibitor analogues.