• 제목/요약/키워드: HPLC Chromatography

검색결과 2,212건 처리시간 0.026초

2002년에서 2004년 동안 서해상공에서 관측된 과산화수소의 농도분포 및 거동 (Distributions and Behaviors of H2O2 Above the Yellow Sea in the Years Between 2002 and 2004)

  • 김영미;신선아;한진석;이미혜;김주애
    • 한국대기환경학회지
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    • 제21권6호
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    • pp.689-697
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    • 2005
  • Hydrogen peroxide is a reservoir of OH radical which is the powerful oxidant in the atmosphere. Therefore, the status of the oxidizing atmosphere could be reflected on the concentration of $H_{2}O_{2}$. In this study, the distribution of $H_{2}O_{2}$ was determined during the intensive aircraft measurements over the Yellow sea in March, December 2002, April, November 2003 and March, October 2004. Flights covered from $124^{circ}E\;to\;129^{circ}E\;and\;35^{circ}N\;to\;37^{circ}N$, and extending to 3,000 m. The flight patterns were set properly to assess the altitudinal and longitudinal distribution for $H_{2}O_{2}$. $H_{2}O_{2}$ was extracted onto aqueous solution using a continuously flowing glass coil and analyzed by a high performance liquid chromatography (HPLC) accompanied with a fluorescence detector using postcolumn enzyme derivatization. Mixing ratios of $O_{3},\;NO_{x}\;and\;SO_{2}$ were measured in real time by commercial analysis instruments. Along the heights, the maximum concentration of $H_{2}O_{2}$ appeared around 1,500 m then gradually decreased with increasing altitude. The vertical behavior of ozone showed the similar trend to $H_{2}O_{2}$. The mean mixing ratio of $NO_{x}$ was about 2 ppbv and not showed clear vertical distribution patterns. The mean value of was the same as $NO_{x}$ however $SO_{2}$ appeared extreme concentration in low altitude. $H_{2}O_{2}\;and\;O_{3}$ showed even longitudinal distribution however $NO_{x}$ mixing ratio in land ($127^{circ}E$) was much higher than over the sea. $SO_{2}$ rather decreased with increasing longitude. $H_{2}O_{2}$ was in inverse proportion to $NO_{x}$ in spring and summer and $SO_{2}$ in spring, which indicated its significant role to NO and $SO_{2}$ oxidation pathways.

액체크로마토그래피를 이용한 농산물중 pyribencarb와 대사물 KIE-9749의 잔류 분석법 (Determination of Pyribencarb and Its Metabolite KIE-9749 in Agricultural Commodities by High-Performance Liquid Chromatography)

  • 권혜영;홍수명;김택겸;김형진;문병철;경기성
    • 농약과학회지
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    • 제20권3호
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    • pp.236-246
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    • 2016
  • 농산물중 pyribencarb와 그 대사물 KIE-9749의 잔류분석법을 개발하였다. 분석법 개발에 사용된 농산물은 5대 작물군의 대표작물인 사과, 고추, 감자, 현미, 대두와 잔류허용기준이 설정된 배, 복숭아, 오이, 포도였다. 각 농산물은 아세톤으로 추출하였으며 액-액분배를 이용하여 1차 정제하고 Florisil solid phase extraction (SPE) cartridge와 aminopropyl SPE cartridge를 이용하여 2차 정제를 실시하는 조건을 확립하였다. 기기분석 조건은 HPLC/UVD 265 nm 파장에서 acetonitrile과 물을 이동상으로 사용하여 확립하였다. 확립된 분석법을 분석자를 달리하여 검증한 결과 pyribencarb의 회수율과 RSD값은 78~108%, 2.7~12.2%였으며, KIE-9749의 회수율과 RSD값은 74~114%와 1.7~15.0%를 보였다. 분석법의 정량한계(LOQ)는 두 성분 모두 $0.05{\mu}g/g$이었으며 LC/ESI-MS/MS를 사용하여 확립된 정성조건에서 방해 피크는 발견되지 않았다. 확립된 분석법은 pyribencarb와 그 대사물 KIE-9749에 대한 농산물의 안전성 검사를 위해 사용될 수 있을 것이다.

포사맥스 정(알렌드론산나트륨 70 mg)에 대한 대웅 알렌드로네이트 정 70 mg의 생물학적동등성 (Bioequivalence of Daewoong AlendronateTM Tablet to FosamaxTM Tablet (Sodium Alendronate 70 mg))

  • 이예리;정선경;양승권;최기호;신용철;전형규;강승우;이희주
    • Journal of Pharmaceutical Investigation
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    • 제36권2호
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    • pp.137-142
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    • 2006
  • A bioequivalence of Daewoong $Alendronate^{TM}$ (Daewoong Pharmaceutical Co., Ltd., Korea) and $Fosamax^{TM}$ tablets (MSD Korea) was evaluated according to the guideline of Korea Food and Drug Administration (KFDA). A single 70 mg dose of sodium alendronate of each medicine was administered orally to 56 healthy male volunteers. This study was performed in a $2\;{\time}\;2$ crossover design. Concentrations of alendronate in the urine were monitored by a high-performance liquid chromatography (HPLC). $A_{et}$ (cumulative urinary excreted amount from time 0 to last sampling interval) was calculated by the accumulation of the urinary excreted alendronate. $U_{max}$ (maximum urinary excretion rate) and $T_{max}$ (time to reach $U_{max}$) were compiled from the urinary excretion rate - time data. Analysis of variance was performed using logarithmically transformed $A_{et}$ and $U_{max}$. No significant sequence effect was found for all of the bioavailability parameters. The 90% confidence intervals of the $A_{et}$ and $U_{max}$ for Daewoong $Alendronate^{TM}/Fosamax^{TM}$ were 0.89-1.12 and 0.82-1.02, respectively. This study demonstrated the bioequivalence of Daewoong $Alendronate^{TM}$ and $Fosamax^{TM}$ with respect to the rate and extent of absorption.

액체크로마토그래프법에 의한 사람 혈장 중 테라조신의 정량 및 테라토닌® 정의 생물학적 동등성 (Determination of Terazocin in Human Plasma by Liquid Chromatography and Bioequivalence Study of Teratonin® Tablets)

  • 조은숙;강성하;전인구
    • Journal of Pharmaceutical Investigation
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    • 제32권2호
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    • pp.119-125
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    • 2002
  • A rapid, selective and reproducible high-performance liquid chromatographic method has been developed for the determination of terazocin in human plasma. Terazocin plus the internal standard, prazocin hydrochloride, were extracted from alkalified plasma with tert-butylmethyl ether, back-extracted into 0.05% phosphoric acid. Fifty ${\mu}l-portions$ of extract were injected onto a octadecylsilane column and eluted with a mixture of acetonitrile, water and triethylamine (30 : 70 : 0.1 v/v, adjusted to pH 5.0 with dilute phosphoric acid) at a flow rate of 1.0 ml/min. The fluorescence intensity of column eluents was monitored at excitation wavelength of 250 nm and emission wavelength of 370 nm. No interference peaks were observed. The practical limit of quantitation was 5 ng/ml for terazocin. The average intraday and interday coefficients of variation were 4.15 and 3.54%, respectively. Also intraday and interday precisions over the range $5{\sim}60\;ng/ml$ were $0.49{\sim}2.92\;and\;0.38{\sim}5.12%$, respectively. The bioequivalence of two terazosin tablets, the $Hytrine^{\circledR}$ (Il Yang Pharmaceutical Co., Ltd.) and the $Teratonin^{\circledR}$ (Sam-A Pharmaceutical Co., Ltd.), was evaluated according to the guideline of Korea Food and Drug Administration (KFDA). Sixteen healthy male volunteers $(24.6{\pm}2.0\;years\;old)$ were divided into two groups and a randomized $2{\times}2$ cross-over study was employed. After one tablet containing 2 mg of terazosin was orally administered, blood was taken at predetermined time intervals and the concentration of terazosin in plasma was determined with a HPLC method using spectrofluorometric detector. AUC was calculated by the linear trapezoidal method. $C_{max}\;and\;T_{max}$ were compiled from the plasma drug concentration-time data. Analysis of variance (ANOVA) was utilized for the statistical analysis of the parameters. The results showed that the differences in $AUC_t,\;C_{max}\;and\;T_{max}$ between the two preparations were 0.21 %, 5.53% and 8.82%, respectively. The powers $(1-{\beta})\;for\;AUC_t,\;C_{max}\;and\;T_{max}$ were >99%, 97.49%, and 33.26%, respectively. Minimum detectable differences $({\Delta},\;%)\;at\;{\alpha}=0.1\;and\;1-{\beta}=0.8$ and the 90% confidence intervals were all less than ${\pm}20%$ except for $T_{max}.\;AUC_t\;and\;C_{max}$ met the criteria of KDFA for bioequivalence, indicating that $Teratonin^{circledR}$ tablets are bioequivalent to $Hytrine^{circledR}$ tablets.

로아큐탄 연질캡슐(이소트레티노인 10 mg)에 대한 니메겐 연질캡슐의 생물학적동등성 (Bioequivalence of NimegenTM Soft Capsule to RoAccutane® Soft Capsule (Isotretinoin 10 mg))

  • 양승권;나숙희;장규영;이윤영;윤미경;유수현;이경률;이희주
    • Journal of Pharmaceutical Investigation
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    • 제37권4호
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    • pp.255-261
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    • 2007
  • A bioequivalence study of $Nimegen^{TM}$ soft capsule (Medica Korea Pharma. Co., Ltd.) to $RoAccutane^{(R)}$ soft capsule (Roche Korea Ind. Co., Ltd.) was conducted according to the guidelines of Korea Food and Drug Administration (KFDA). Thirty healthy male Korean volunteers received each medicine at the isotretinoin dose of 60 mg in a $2{\times}2$ crossover study. There was one week wash-out period between the doses. Plasma concentrations of isotretinoin were monitored by a high performance liquid chromatography (HPLC) for over a period of 48 hours after drug administration. $AUC_t$ (the area under the plasma concentration-time curve from time zero to 48 hr) was calculated by the linear trapezoidal rule method. $C_{MAX}$ (maximum plasma drug concentration) and $T_{MAX}$ (time to reach $C_{MAX}$) were compiled from the plasma concentration-time data. Analysis of variance was carried out using logarithmically transformed $AUC_t\;and\;C_{MAX}$. No significant sequence effect was found for all of the bioavailability parameters indicating that the crossover design was properly performed. The 90% confidence intervals of the $AUC_t$ ratio and the $C_{MAX}$ ratio for $Nimegen^{TM}/RoAccutane^{(R)}$ were $log0.860{\sim}log0.98\;and\;log0.85{\sim}log1.00$, respectively. These values were within the acceptable bioequivalence intervals of $log0.80{\sim}log1.25$. Thus, our study demonstrated the bioequivalence of $Nimegen^{TM}\;and\;RoAccutane^{(R)}$ with respect to the rate and extent of absorption.

능이버섯(Sarcodon aspratus)으로부터 분리한 diketopiperazine계 화합물의 화학구조 및 항산화활성 (Structures and Antioxidant Activity of Diketopiperazines Isolated from the Mushroom Sarcodon aspratus)

  • 김진우;문병식;박영민;유남희;유인자;;유익동;김종평
    • Applied Biological Chemistry
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    • 제48권1호
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    • pp.93-97
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    • 2005
  • 능이버섯(Sarcodon aspratus) 자실체의 MeOH 추출물을 n-hexane, EtOAc, n-BuOH 및 물로 추출하였다. 이 중 프리라디칼 소거활성을 나타내는 EtOAc 분획을 silica gel 및 Sephadex LH-20 column chromatograpy를 실시한 후 $C_{18}$ HPLC를 통해 프리라디칼 소거활성을 나타내는 3종의 항산화 활성물질 Sa-1, Sa-2 및 Sa-3를 분리하였다. 각 화합물의 구조를 NMR 및 MS 등의 스펙트럼 데이터를 분석하여, diketopiperazine계 화합물들인 cyclo(prolyl-valyl), cyclo(prolyl-leucyl) 및 cyclo(prolyl-isoleucyl)로 동정하였다. 이 화합물들은 능이버섯으로부터 최초로 분리되었으며, 이들의 항산화 활성을 측정한 결과 DPPH radical 소거활성$(EC_{50}\;0.15{\sim}0.18\;mM)$ 및 superoxide radical 소거활성$(EC_{50}\;0.21{\sim}0.24\;mM)$을 나타내었다.

갈화의 Prolyl Endopeptidase 저해 활성 Isoflavonoid 및 이들의 $^{13}C-NMR$ Assignment (Prolyl Endopeptidase-inhibiting Isoflavonoids from Puerariae Flos and Some Revision of their $^{13}C-NMR$ Assignment)

  • 김경범;김상인;김종식;송경식
    • Applied Biological Chemistry
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    • 제42권4호
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    • pp.351-355
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    • 1999
  • 갈화로부터 항치매 효과를 기대할 수 있는 prolyl endopeptidase(PEP) 저해제를 분리하기 위하여 갈화의 methanol 추출물을 chloroform 및 ethyl acetate로 분배추출 후 chloroform 가용성 분획에 대하여 silica gel, Sephadex LH-20 column chromatography 및 RP-HPLC를 행한 결과, $FeCl_3$,에 양성 반음을 나타내는 4종의 화합물을 얻었다. 이들을 $^1H-$, $^{13}C-$, $^2D-NMR$ 및 MS 등을 이용하여 분석한 결과, 각각 tectorigenin, genistein, 5,7-dihydroxy-4',6-dimethoxyisoflavone, 5-hydroxy-6,7,4'-trimethoxyisoflavone으로 동정하었으며 HMBC, HMQC를 통하여 $^{13}C-NMR$ signal들을 assign함으로써 기 보고된 data들의 오류를 바로잡았다. PEP에 대한 이 화합물들의 $IC_{50}$값은 각각 5.30 ppm$(17.7\;{\mu}M)$, 10.39 ppm$(38.5\;{\mu}M)$, 13.92 ppm$(44.3\;{\mu}M)$, 20.61 ppm$(62.8\;{\mu}M)$이었다.

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된장에서 분리한 Bacillus sp. BCNU 9171에 의한 바이오제닉 아민 생산 저해 (Inhibition of Biogenic Amine Production by Bacillus sp. BCNU 9171 Isolated from Doenjang)

  • 박여진;주우홍
    • 한국미생물·생명공학회지
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    • 제45권4호
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    • pp.299-304
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    • 2017
  • Histamine, tyramine, cadaverine 및 putrescine과 같은 바이오제닉 아민은 소비자의 건강에 해로운 영향을 줄 수 있으므로 식품에서 독성 물질로 관리되어야 한다. 최근 몇 년 동안, 바이오제닉 아민을 분해할 수 있는 미생물의 적용은 바이오제닉 아민 함량의 감소를 위한 새로운 방법이 되고 있다. 먼저 Bacillus sp. BCNU 9171 균주를 한국 전통발효 된장으로부터 분리하였다. 4개의 아민 생성 식중독 세균들에 의한 바이오제닉 아민 생산에 대한 Bacillus sp. BCNU 9171의 배양 상등액(CFS)의 저해율을 HPLC를 사용하여 조사하였다. 본 실험 결과는 10% (1 ml + 9 ml HDB), 25%(2.5 ml CFS + 7.5 ml HDB), 50% (5 ml CFS + 5 ml HDB) 및 75% (7.5 ml CFS + 2.5 ml HDB)의 네 가지 CFS 농도가 대조군에 비해 4가지 아민 생성균에 대한 바이오제닉 아민 생산을 87%까지 감소시켰음을 보여주고 있다. 이 결과는 아민 생성균에 의한 발효 식품에 의한 다량의 바이오제닉 아민이 축적되는 것을 막기 위해 발효식품 및 식품 안전용으로 Bacillus sp. BCNU 9171를 starter 균주로 이용 가능하다는 것을 보여주고 있다.

동백나무 잎 용매분획물의 항산화 및 항암 활성 (Antioxidative and Anticancer Activities of Various Solvent Fractions from the Leaf of Camellia japonica L.)

  • 김진희;정창호;심기환
    • 한국식품저장유통학회지
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    • 제17권2호
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    • pp.267-274
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    • 2010
  • 동백나무 잎을 새로운 기능성 식품의 재료로 활용하기 위하여 항산화 및 항암활성을 측정한 결과는 다음과 같다. DPPH radical 소거활성을 측정한 결과 분획물의 농도가 증가함에 따라 DPPH radical 소거활성이 증가하는 경향을 보였으며, 특히 물 분획물에서 가장 높은 DPPH radical 소거활성을 보였다. 환원력도 분획물의 농도가 증가함에 따라 환원력이 증가하는 경향을 보였으며, 환원력 또한 물 분획물에서 가장 높게 나타났다. Linoleic acid를 이용한 자동산화 억제활성을 실험한 결과 다른 분획물에 비하여 물 분획물에서 가장 높은 과산화 억제활성을 나타내었고, 분획물의 농도가 증가함에 따라 아질산염 소거활성 역시 증가하는 경향을 보였으며, 특히 부탄올 및 물 분획물을 $1,000{\mu}g/mL$의 농도로 첨가하였을 때 각각 92.15%와 95.61%의 높은 아질산염 소거활성을 보였다. 폐암세포와 결장암세포에 대한 생육억제활성을 측정한 결과 부탄올 및 물 분획물에서 가장 높은 생육억제활성을 보였다. 총 페놀릭 화합물은 부탄올 및 물 분획물에서 각각 216.26 및 220.68 mg/g으로 나타났으며, HPLC로 물 분획물의 페놀릭 화합물을 분석한 결과 quercetin과 epicatechin이 가장 많이 함유되어 있었고, 동백나무 잎의 항산화 및 항암활성은 quercetin과 epicatechin과 같은 폴리페놀 화합물에 의한 것으로 추측된다.

4-Tert-Octylphenol의 랫드에서의 조직분포 및 독성동태에 관한 연구 (Tissue Distribution and Toxicokinetics of 4-Tert-Octylphenol in Rats)

  • 강미경;안미령;정혜주;최선옥;최홍석;양지선;이용복;유태무;손수정
    • Toxicological Research
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    • 제20권3호
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    • pp.195-203
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    • 2004
  • 4-Tert-Octylphenol (OP) is a surfactant additive widely used in the manufacture of a variety of detergents and plastic products. OP can disrupt endocrine function in humans and animals. This study was carried out to obtain toxicokinetic parameters of OP in male Sprague-Dawley (SD) rats. Male rats were administered with OP by single oral application of 200 mg/kg body weight. Blood, urine and tissues samples were taken at several time intervals after administration. Analysis of samples for OP was performed by column-switching high performance liquid chromatography (HPLC). In addition, we exam-ined tissue distribution and accumulation of OP after single oral application of 50, 100, and 200 mg/kg, single intravenous injection of 1, 5 and 10 mg/kg or daily application of 50 mg/kg for 14 consecutive days. After single oral administration of 200 mg/kg, Cmax of 213 $\pm$ 123 ng/ml was reached within the first 1.3 hr (Tmax) in the plasma. AUC was calculated for 1,333$\pm$484 ngㆍhr/ml. The final elimination half-life of plasma was longer than that of urine, but urinary clearance was lower than oral. A very small fraction of OP (Fe < 0.0017%) was excreted in urine within 24 hr. These results indicated that the major excretion route of OP was not urine. The mean maximal tissue distribution of OP was obserbed at 6 hr after treatment and slowly decreased time-dependently. High OP concentrations were detected in fat at 24 hr. The OP in fat was slowly released with longer elimination half-life and lower clearance than that of other tissues. OP was not accumulated in the liver following single oral application but 14-day oral treatments resulted in two-fold accumulation. It was probably due to the saturation of detoxification pathways. On the other hand, the mRNA expression of cytochrome P450 isoforms except CYP2C11 was not affected by OP at any dose. The expression of CYP2C11 mRNA decreased in a dose-dependent manner. This result suggests that OP changes expression of the male-specific cytochrome P450 isoforms in rat liver, and these changes are closely related to the toxic and estrogenic effect of OP.