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GC/FPD를 利用한 ${\beta}$-락탐系 抗生物質의 分析(II)
박만기,조영현,양정선,박정일,Park, Man-Ki,Cho, Yung-Hyun,Yang, Jeong-Seon,Park, Jeong-Hil 대한약학회 1984 약학회지 Vol.28 No.4
For gas chromatographic determination with the sulfur-specific flame photometric detector, nine ${\beta}$-lactam antibiotics without ${\alpha}$-amino group were esterified with borontrifluoride-methanol complex and then N-benzoylated with benzoyl chloride. The gas chromatographic separation of these products was successfully carried out on various silicon polymers (OV-1, OV-101, OV-17, OV-225, and QF-1) coated on the acid washed, silanized diatomite. The structure of the esterified and N-benzoylated product was confirmed by mass spectromer.
NMR Spectroscopy에 의한 Sulfonamide의 정량(定量)
박만기,김성경,이숙연,Park, Man-Ki,Kim, Sung-Kyeong,Lee, Sook-Yeon 대한약학회 1984 약학회지 Vol.28 No.5
A rapid and accurate NMR procedure for the analysis of a mixture of sulfametrol, sulfalene and sulfameter in $CDCl_3$ and $dimethylsulfoxide-d_6$ was developed. Thioacetamide was used as an internal standard. The signals chosen for the analysis were a singlet of 4.03ppm due to the methoxyl group of sulfametrol, a singlet of 3.98ppm due to the methoxyl group of sulfalene and a singlet of 3.83ppm due to the methoxyl group of sulfameter. The quantification of the characteristic peak was done by the integration method and the peak height method. The variation coefficient of sulfametrol, sulfalene and sulfameter were 1.7(n=6), 1.7(n=6) and 1.4%(n=6), respectively in the peak height method and 8.9(n=6), 9.4(n=6) and 7.0(n=6), respectively in the integration method.
아미노산 Phenylthiohydantoin 유도체를 키랄 고정상으로 한 GC에 의한 아미노산 광학 이성질체의 상호분리
박만기,양정선,고창범,이미영,Park, Man-Ki,Yang, Jeong-Seen,Ko, Chang-Bum,Lee, Mi-Yung 대한약학회 1988 약학회지 Vol.32 No.3
The resolution of five amino acids derivatives by gas chromatography on phenylthiohydantoin derivatives as chiral stastionary phase was investigated. (S)-5-isopropyl, isobutyl, (sec)-butyl and benzoyl derivatives of $N^3-phenyl-2-thiohydantoin$ were synthesized from L-valine, L-leucine, L-isoleucine and L-phenylalanine, respectively. The phases were employed at several column temperatures ($140^{\circ}C{\sim}210^{\circ}C$). The separation factors were compared with each stationary phase with varying R groups. The possible mechanism of chiral recognition was investigated by NMR technique.
박만기(Man Ki Park),박정일(Jeong Hill Park),김용철(Yong Chul Kim),한병훈(Byung Hoon Han),한용남(Yong Nam Han),류재하(Jae Ha Ryu),유승조(Seung Jo Yoo),김경호(Kyoung Ho Kim) 한국생약학회 1989 생약학회지 Vol.20 No.2
The alkaloids of thirty five Korean plants which belong to Rhamnaceae, Sterculiaceae, Celastracea, Urticaceae and Rubiaceae were screened. Plant was extracted and solvent fractionated to yield ether soluble alkaloidal fraction and butanol soluble fraction. Each fraction was subjected to alkaloidal test by Dragendorff`s reaction. The result showed eighteen plants strong positive, fourteen weak and six negative to alkaloidal test.
생약 중 잔류 생약의 분석법: GC/MS 에 의한 27종 잔류 규제 농약의 분석
박만기(Man Ki Park),박정일(Jeong Hill Park),윤혜란(Hye Ran Yoon),윤인병(In Byoung Yoon),조술연(Sool Yeon Cho),황귀서(Gwi Seo Hwang) 대한약학회 1996 약학회지 Vol.40 No.2
GC/MS analysis of 27 controlled pesticides in herbal drugs was studied. Selected ion monitoring(sim) technique was applied to increase the GC/MS sensitivity. Typical peaks in the mass spectrum of each pesticides were selected as quantitation, comfirmation or alternate ion. Twenty seven pesticides were divided into five groups according to their retention time and the peaks for SIM were programmed accordingly. The combination of two ionization methods, electron impact(EI)-SIM-MS and negative ion chemical ionization(NCI)-SIM-MS, were well-fitted for the detection, confirmation and quantitation of multiclass residual pesticides in herbal drugs.
가스 크로마토그래피에 의한 아민노산 광학 이성질체의 분리(III) (S)-5-isobutyl-N3-phenyl-2-thiohydantoin의 광학 활성 고정상으로의 응용
박만기(Man Ki Park),양정선(Jeong Seon Yang),고창범(Chang Bum Ko) 대한약학회 1988 약학회지 Vol.32 No.2
The resolution of N-trifluoroacetyl(N-TFA) ter-isopropylesters of Ala, Ile, Leu, Val and Phe by gas chromatography on the (S)-5-isobutyl-N3-phenyl-2-thiohydantoin as stationary phase was investigated. The phase was employed at several column temperatures(140oC-200oC) and the separation factors were 1.18-1.45 range for five amino acid enantiomers. The possible mechanism of chiral recognition was investigated by NMR technique and the association constant(Kc) was calculated as 201.3(r=0.98) for alanyl derivative.
박만기(Man Ki Park),박정일(Jeong Hill Park),김경호(Kyoung Ho Kim),한상범(Sang Bum Han),한병훈(Byung Hoon Han) 대한약학회 1994 약학회지 Vol.38 No.4
Eight aromatic acids in Panax ginseng were determined by GC. Ultra- 1 (25mX0.2mmX0.33mcm) capillary column was employed with temperature programming from 150oC to 240oC at a rate of 3oC/min. The mean contents of eight aromatic acids in 8 white ginseng samples were as follows; salicylic acid: 4.30ppm, cinnamic acid: 18.2ppm, vanillic acid: 4.22ppm, gentisic acid: trace, syringic acid: 6.69ppm, p-coumaric acid: 13.3ppm, ferulic acid: 21.9ppm, caffeic acid: 24.3ppm, respectively.
박만기(Man Ki Park),김종문(Jong Moon Kim),황귀서(Gwi Seo Hwang) 대한약학회 1996 약학회지 Vol.40 No.1
Chemical constituents of Uncaria hooks were studied. Four compounds were isolated from the ether soluble fraction by chromatographic purification process. They were identified as isocorynoxeine-N-oxide, anti-isorhynchophylline-N-oxide, physcion and ursolic acid by spectral evidences. Their contents analyzed by HPLC or GC method were physcion 0.04%, ursolic acid 0.26%, isocorynoxeine-N-oxide 0.04% and anti-isorhynchophylline-N-oxide 0.03% respectively. Isocorynoxeine-N-oxide was not reported in nature so far.
박만기(Man Ki Park),박정일(Jeong Hill Park),김경호(Kyeong Ho Kim),신영근(Young Geun Shin),명경민(Kyung Min Myoung),이종호(Jong Ho Lee) 한국생약학회 1995 생약학회지 Vol.26 No.3
Two compounds were newly isolated from the leaf exudates of Aloe capensis and identified as 10-C-rhamnosyl aloe-emodin anthrone and aloenin B, on the basis of chemical and spectroscopic evidences.