LC-ESI-MS/MS를 이용한 생체시료 중 브롬화피나베리움의 고감도 분석 및 이를 이용한 생체이용률 평가 : Applicability to Oral Bioavailability Determination

박석,이예리,김호현,이희주,김윤균,염정록,한상범 한국약제학회 2004 Journal of Pharmaceutical Investigation Vol.34 No.6

A sensitive method for quantification of pinaverium bromide in human plasma was established using liquid chromatography-electrospray ionization tandem mass spectrometrv(LC-ESI-MS/MS). Glimepiride was used as internal standard. Pinaverium bromide and internal standard in plasma sample were extracted using tert-but}lmethvlether(TBME). A centrifuged upper laver was then evaporated and reconstituted with mobile phase of acetonitrile-5 m1VI ammonium formate (8020. pH 3.0). The reconstituted samples were injected into a C_(18) reversed-phase column. Using MS/MS with multiple reaction monitoring (MRM) mode. pinaverium and glimepirde were detected without severe interference from human plasma matrix. Pinaverium produced a protonated precursor ion ([M+H]^(+)) at m/z 510.3 and a corresponding product ion at m/z 228.9. Internal standard produced a protonated precursor ion ([M+H] ^(+)) at m/z 491.5 and a corresponding product ion at m/z 352.0. Detection of pinaverium bromide in human plasma was accurate and precise. with limit of quantitation at 0.5 ng/ml. The method has been successfully applied to bioavailability study of pinaverium bromide tablet in Korean healthy male volunteers. Pharmacokinetic parameters such as AUCr. C_(max) T_(max). K_(el) and t_(l/2) were calculated.

건강한 한국인 성인 남성에서 레보설피리드 제제의 생체이용률

이정민,최성업,김희규,윤미경,김세희,염정록,최영욱 한국약제학회 2003 Journal of Pharmaceutical Investigation Vol.33 No.3

Pharmacokinetics and oral bioavailability of levosulpiride was determined in Korean healthy male volunteers. Thirty subjects received a single oral dose (25 ㎎) of a tablet in randomized 2×2 cross-over design. The plasma concentratons of levosulpiride were measured by HPLC and compared with those reported in the literature. Pharacokinetic parameters for Isomeric^(??) tablet (levosulpiride 25 ㎎) were revealed as follows: AUC _(inf) 737.1±176.9 ng·hr/ml, C_(max) 56.4±20.1 ng/ml, T_(max) 4.2±1.6hr, K_(a) 1.00±1.09 hr^(-1), K_(el) 0.08±0.02 hr^(-1), and t_(1/2) 8.8±1.9 hr. The rate constant of the absorption phase was obtained based on the first-order kinetics. In the aspect of bioavailability, Isomeric^(??) tablet was bioequivalent to the other product (Levopride^(?)tablet) available in the Korean market. Intersubject variations and race differences were shown in comparison with the published date in the literature, even though there ws a linear relationship between dose and extent of bioavailability.

13C NMR 화학 Shift 측정에 미치는 TMS의 거동

염정록(Jeong Rok Youm) 대한약학회 1989 약학회지 Vol.33 No.3

A method is presented for calculating the 13C chemical shifts produced in liquid solution by referenced relative to RF frequency. The method is useful to get the real variations of chemical shifts in magnetic field by eliminating the affects of the variation of a reference substance.

alpha-치환 톨루엔 유도체의 13C NMR 화학 Shift

염정록(Jeong Rok Youm) 대한약학회 1988 약학회지 Vol.32 No.3

13C NMR chemical shifts for 18 alpha-susbstituted toluenes at high dilution in CCl4 solution have been determined. Substituents are as follows: H, Me, Et, n-Pr, iso-Pr, Ph, F, Cl, Br, NH2, NHMe, NMe2, OH, OMe, OCOMe, C02Me, C02Et, CN. Those chemical shifts of the methylene carbon of the toluene and the alpha-carbon of the n-butane systems are correlated well. (r=.975, slope=.962)

앉은부채(Symplocarpus renifolius Schott) 뿌리의 성분

염정록,박동우,Youm, Jeong-Rok,Park, Dong-Woo 한국생약학회 1997 생약학회지 Vol.28 No.3

From the root of Symplocarpus renifolius, four compounds were isolated and their structure was elucidated by chemical and spectroscopic methods. They were identified as ${\beta}-sitosterol$ (compound 1), asparagine (compound 2), isocorydine (compound 3) and 3-hydroxymethyl-4-phenyl phenoxy carboxylic acid glucopyranosyl ester (compound 4). These compounds were firstly isolated from roots of Symplocarpus renifolius. Compound 4 was identified as a new compound, named as symplocarposide.

Enoxacin의 Dansyl 유도체에 의한 형광광도 분석법

이경준,염정록 중앙대학교 약학연구소 1990 약학 논총 Vol.4 No.-

A sensitive and specific method is described for the determination of a new secondary aromatic amine chemotherapeutic drug, Enoxacin. The highly fluorescent Dns-derivative of Enoxacin has been obtained by reacting ethanol solution of Enoxacin with Dns-Cl in acetone and sodium bicarbonate aqueous solution. The Dns-derivative is extracted with methylene chloride and its concentration is measured using a spectrofluorimeter in methanol solution(excitation wavelength : 415nm, emission wavelength : 535nm). The amount of Dns-Cl and 0.1M-NaHCO_3, reaction temperature, reaction time, stability of Dns-derivative and extraction solution were investigated to determine the quantitative potential of the method. Limit of detection is 0.1㎍ / ml with linear response up to 8㎍ / ml and 40㎍ / ml(as Enoxacin in methanol). The fluorescent labelled method is very stable and applicable to the determination of Enoxacin contained in pharmaceutical preparation.

Analysis of Oxaprozin and its Metabolites in human Urine by High Performance Liquid Chromatography and Solid Phase Extraction

Kwon, Min-Chang,Youm,Jeong-Rok 중앙대학교 약학연구소 1996 약학 논총 Vol.10 No.-

A new sensitive and simple method for the rapid. simultaneous pretreatment of oxaprozin and its hydroxy oxaprozin metabolites, in human urine is described. Reversed-phase High-Performance Liquid Chromatography (HPLC) employed a Cosmosil C_18 column using acetonitrile-deionized water adjusted to pH 3.25 with acetic acid as a gradient mobile phase with ultraviolet detection at 280 nm. It is essential that urine is handled rapidly and acidified upon collection prior to freezing in order to stabilize the metabolites. Urine samples first are centrifuged and oxaprozin, hydroxy oxaprozin metabolites are initially isolated by solid-phase extraction on "Waters" C_18 disposable extraction columns for sample clean-up. Upon elution, the residue is evaporated, dissolved in indomethacin (internal standard) solution and injected onto the HPLC system. One of the metabolites of oxaprozin, hydroxy oxaprozin metabolites, extracted by SPE from urine was identified by electrospray ionization mass spectrometry. The above methods are satisfactory for the analysis of oxaprozin and its metabolites in human biological fluids.

Biphenyldimethyldicarboxylate 및 그 가수분해물의 온도에 의한 Chemical Shift의 거동

김진수,염정록 중앙대학교 약학연구소 1994 약학 논총 Vol.8 No.-

The temperature dependence of ^13C and ^1H nuclear magnetic resonance in biphenyldimethyldicarboxylate(PMC) and its hydrolysate have been investigated. The ^13C and ^1H chemical shifts of PMC and its hydrolysate is shown to be temperature dependent. Most of all, influence of its structure is the major factor on linear correlation between chemical shift and temperature. In solvent effect, PMC in CDCl_3 and DMSO-d_6 showed different chemical shifts and NMR spectrum patterns, respectively.

Rapid HPLC Method for the Simultaneous Determination of Eight Urinary Metabolites of Toluene, Xylene and Styrene

Lee, Cheol-Woo,Lee, Jeong-Mi,Lee, Jae-Hyun,Eom, Han-Young,Kim, Min-Kyung,Suh, Joon-Hyuk,Yeom, Hye-Sun,Kim, Un-Yong,Youm, Jeong-Rok,Han, Sang-Beom Korean Chemical Society 2009 Bulletin of the Korean Chemical Society Vol.30 No.9

Toluene, xylene and styrene are volatile organic solvents that are commonly used in mixtures in many industries. Because these solvents are metabolized and then excreted in urine, their urinary metabolites are thought to be biomarkers of occupational exposure to these solvents. Therefore, a simple, rapid, and yet reliable analytical method for determining the metabolites is required for accurate biological monitoring. In the present study, a simple and rapid HPLC-UV method was developed for the simultaneous determination of eight major metabolites of toluene, xylene and styrene: hippuric acid (HA), mandelic acid (MA), o-, m- and p-methylhippuric acids (o-, m- and p-MHAs), and o-, m- and p-cresols. A monolithic column was employed as the stationary phase and several conditions, including flow rate, composition of mobile phase and column temperature, were variables for the optimization of the chromatographic resolution. All eight metabolites were successfully resolved within 5 minutes in 10% aqueous ethanol containing 0.3% acetic acid and 1.6% $\beta$-cyclodextrin, using a flow rate gradient of 1.0 - 5.0 mL/min at 25 ${^{\circ}C}$. The performance of this method was validated by linearity, intra- and inter-day accuracy, and precision. The linearity was observed with correlation coefficients of 0.9998 for HA, 0.9999 for MA, 0.9989 for o-MHA, 0.9998 for m-MHA, 0.9991 for p-MHA, 0.9997 for o-cresol, 0.9998 for m-cresol, and 0.9986 for p-cresol. The intra- and inter-day precision of the method were less than 5.89% (CV) and the accuracy ranged from 92.95 to 106.62%. The validity was further confirmed by analysis of reference samples that were prepared by the inter-laboratory quality assurance program of the Korea Occupational Safety and Health Agency (KOSHA, Seoul, Korea). All measured concentrations of the analytes agreed with the certified values.

Cephalosporin의 정량적 구조-활성 상관관계 : 7β-Acyl Amino Side Chain α-Carbon 치환 유도체 Substituted Compounds of 7β-Acyl Amino Side Chain α-Carbon

박인철,염정록 중앙대학교 약학연구소 1992 약학 논총 Vol.6 No.-

The QSAR(Quantitative Structure-Activity Relationship) of twenty-five cephalosporins were studies to evaluate the importance of the permeability of cephalosporins through the cell wall of gram negative bacteria and the affinity of cephalosporins for cephalosporin binding protein. The permeability was affected by steric volume rather than hydropyobicity of cephalosporins and the antibiotic activity was affected by affinity rather than permeability. As a result, introduction of hydrogen binding group at 7B-acyl amino side chain a-carbon is essen-tial to new cephalosporins. In addition to, the imporvement of permeability of cephalosporins, which might be enhanced by introducing positive charge into molecule and reducing steric volume, is important.