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LC-MS/MS를 이용한 돼지 근육 및 신장에서 8종 페니실린계 항생물질의 동시잔류분석법
임채미 ( Chae Mi Lim ),권현정 ( Hyun Jeong Kwon ),조병훈 ( Byung Hoon Cho ),박수정 ( Su Jeong Park ),정갑수 ( Gap Su Chung ),손성완 ( Seong Wan Son ) 한국예방수의학회(구 한국수의공중보건학회) 2011 예방수의학회지 Vol.35 No.4
A rapid, simple and reliable LC-MS/MS method, which can be used on a routine basis, was developed for the simultaneous detection of 8 penicillin antibiotics (amoxicillin, ampicillin, penicillin-G, penicillin-V, oxacillin, cloxacillin, nafcillin and dicloxacillin) in swine muscle and kidney. The antibiotics were extracted from samples with water and methanol. The extract was centrifuged, filtered and analyzed by liquid chromatography coupled with a tandem mass spectrometer (LC-MS/MS), using a C18 reversed phase column with water/acetonitrile gradient containing 0.05 % formic acid. Mass spectral acquisition was achieved in an electrospray positive ion mode by applying multiple reaction monitoring (MRM) of 2 fragment ion transitions to provide a high degree of sensitivity and specificity. The ion rations were consistent and could be used for confirmation of identity of the penicillin antibiotics. Recoveries of eight penicillins at three fortification levels (10, 20 and 40㎍/㎏) ranged from 79.8 to 102.4% and 72.8 to 103.4% in swine muscle and kidney, respectively. The coefficient of variation was than 9% in all samples. The estimated limits of quantification (LOQs) ranged from 1.0 to 3.2㎍/㎏in swine muscle and kidney, respectively. The LOQs of this method are below the MRLs of penicillin antibiotics in animal tissues established in Korea and other countries.
LC-MS/MS를 이용한 우유 중 설파제의 동시 잔류 분석법
임채미 ( Chae Mi Lim ),권현정 ( Hyun Jeong Kwon ),조병훈 ( Byung Hoon Cho ),박수정 ( Su Jeong Park ),정갑수 ( Gap Su Chung ),손성완 ( Seong Wan Son ) 한국수의공중보건학회 2010 예방수의학회지 Vol.34 No.3
A simple, selective and sensitive procedure for the confirmation of 14 sulfonamide antibacterials in milk was developed. The milk samples were homogenized, extracted and deproteinized by acetonitrile and defatted by n-hexane. Analysis was performed by liquid chromatography with tandem mass spectrometry (LC-MS/MS) in positive mode for all 14 analytes. Mass spectral acquisition was performed in the multi reaction monitoring mode (MRM), selecting two structurally significant transitions per compound. The calibrations were performed in sample matrixes and the interference effect of sample matrixes on the ionization was effectively eliminated. Good linear relationship (R2=0.992~0.999) were observed at 6 concentrations of 2.5~100 ng/g. Satisfied recoveries (86.3~110.2%) of all sulfonamides were demonstrated in spiked milk at three levels from 5 to 20 ng/g. The limits of quantitation (LOQs) for sulfonamides ranged from 0.25~2.1 ng/g.
원저 : LC-MS/MS를 이용한 돈육에서 퀴놀론계 약물의 동시 잔류 분석법
임채미 ( Chae Mi Lim ),권현정 ( Hyun Jeong Kwon ),조병훈 ( Byung Hoon Cho ),박수정 ( Su Jeong Park ),정갑수 ( Gap Su Chung ),손성완 ( Seong Wan Som ) 한국수의공중보건학회 2010 예방수의학회지 Vol.34 No.4
A reversed-phase high-performance liquid chromatography with tandem mass-spectrometric detection was developed and validated for the simultaneous analysis of 13 quinolones (orbifloxacin, sarafloxacin, marbofloxacin, ofloxacin, enrofloxacin, danofloxacin, pefloxacin, ciprofloxacin, norfloxacin, difloxacin, oxolinic acid, flumequine, nalidixic acid) in pork. The drugs were extracted from homogenized sample using acidic buffer (2% trichloracetic acid) and acetonitrile with ethyl acetate. Analysis was performed by liquid chromatograph with tandem mass spectrometry (LC-MS/MS) in positive mode for all quinolones. Mass spectral acquisition was performed in the multi reaction monitoring mode (MRM), selecting two structurally significant transitions per compound. Good linear relationship (R2=0.999) was observed at 6 concentrations of 2.5~100 ng/g. Satisfied recoveries (73.3~105.4%) of all quinolones were demonstrated in spiked pork at three levels from 5 to 20 ng/g. The limits of quantitation (LOQs) for quinolones ranged from 0.25 to 5.0 ng/g.