• 제목/요약/키워드: Liquid chromatography- fluorescence detector

검색결과 71건 처리시간 0.037초

Bioequivalence Assessment of Roxithromycin Tablets in Healthy Korean Volunteers

  • Kwon Oh-Seung;Kim Hye-Jung;Pyo Hee-Soo;Chung Youn-Bok
    • Biomolecules & Therapeutics
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    • 제14권1호
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    • pp.50-55
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    • 2006
  • The objective of the study was to evaluate the bioequivalency between the $Rozid^{TM}$ Tablet (Ilhwa Pharm. Co., Ltd.) as a test formulation and the $Rulid^{TM}$ Tablet (Handok Pharm. Co., Ltd) as a reference formulation. Twenty-four healthy male volunteers were administered the formulations by the randomized Latin square crossover design, and the plasma samples were determined by a high performance liquid chromatography (HPLC) with fluorescence detector. $AUC_t,\;C_{max}\;and\;T_{max}$ were obtained from the time-plasma concentration curves, and log-transformed $AUC_t\;and\;C_{max}$ and log-untransformed $T_{max}$ values for two formulations were compared by statistical tests and analysis of variation. $AUC_t$ was determined to be $63.30{\pm}25.57{\mu}g.hr/ml$ for the test formulation and $64.02{\pm}29.27mg.hr/ml$ for the reference formulation. The mean values of $C_{max}$ for the test and reference formulations were $5.07{\pm}2.14\;and\;5.53{\pm}2.60{\mu}g/ml$, respectively. The $AUC_t,\;and\;C_{max}$ ratios of the test $Rozid^{TM}$ Tablet to the reference $Rulid^{TM}$ Tablet were -1.12% and -8.32%, respectively, showing that the mean differences were satisfied the acceptance criteria within 20%. The results from analysis of variance for log-transformed $AUC_t,\;and\;C_{max}$ indicated that sequence effects between groups were not exerted and 90% confidence limits of the mean differences for $AUC_t,\;and\;C_{max}$ were located in ranges from log 0.80 and log 1.25, satisfying the acceptance criteria of the KFDA bioequivalence. The RozidTM Tablet as the test formulation was considered to be bioequivalent to the RulidTM Tablet used as its reference formulation, based on $AUC_t,\;and\;C_{max}$ values.

Discrimination of Ginseng Habitat by Using Instrumental Analysis Techniques

  • Sohn H. J.;Lee S. K.;Cho B. G.;Kim S. J.;Lee N. Y.;Choi D. S.;Jeong M. S.;Bae H. R.;Yang J. W.
    • 고려인삼학회:학술대회논문집
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    • 고려인삼학회 2002년도 학술대회지
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    • pp.238-252
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    • 2002
  • In order to screen out indicators for the discrimination of ginseng habitat, some physical and chemical characteristics of Korean red ginsengs (94 kinds) and Chinese red ginsengs (50 kinds) were analyzed by using a rheometer, an electronic nose system, a combined technique of solid phase micro-extraction (SPME) and gas chromatograph equipped with an electron capture detector (GC/ECD), an X-ray fluorescence spectrometer (XRF), an inductively coupled plasma mass spectrometer (ICP/MS), a near infrared spectrometer (NIRs) and high performance liquid chromatography equipped with evaporative light scattering detector (HPLC/ELSD). The results are summarized as follows: (i) The rhizome strengths of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. (ii) The electronic nose patterns of Korean red ginsengs were significantly different from those of Chinese red ginsengs. (iii) Some unidentified peaks were detected not in the headspace of Korean red ginsengs but in the headspace of Chinese red ginsengs when the headspace volatiles prepared by the SPME technique were analyzed by GC/ECD. (iv) Either the content ratios of K to Ca or Mn to Fe were significantly different between Korean red ginsengs and Chinese red ginsengs. (v) The reflectance ratios of NIRs wavenumbers such as $904\;cm^{-1}\;to\;1088\;cm^{-1}$ for Korean red ginsengs were significantly different from those for Chinese red ginsengs. (vi) The content ratios of ginsenoside-Rg to ginsenoside-Re of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. These results indicate that the rhizome strength, the electronic nose pattern, the occurrence of ECD-sensitive headspace volatile components, the content ratios of K to Ca and Mn to Fe, the NIRs pattern and the content ratio of ginsenoside-Rg to -Re may be indicators for the discrimination of ginseng habitat.

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액체크로마토그래피-형광검출기를 이용한 닭고기 중 플루오로퀴놀론계 항균물질 정량분석 및 잔류조사 (Determination and Survey of Fluoroquinolones Residue in Chicken Muscle by HPLC with Fluorescence Detector)

  • 박은정;임지흔;이성모
    • 한국식품위생안전성학회지
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    • 제19권1호
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    • pp.12-18
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    • 2004
  • 1. 닭고기에서 4종의 플루오로퀴놀론계 합성항균제(ofloxacin, norfloxacin, ciprofloxacin, enrofloxacin)를 액상추출법으로 추출하여 형광검출기와 HPLC를 이용하여 동시 정량 분석하는 방법을 확립하였으며 분석조건으로서 컬럼은 Symmetry Cl8(250${\times}$4.6 mm id, 5 $\mu\textrm{m}$), 이동상은 0.4% triethylamine 및 0.4% phospholic acid 수용액, methanol 및 acetonitrile 혼합용액(800: 100: 100, v/v/v)을 사용하였으며, 형광검출기는 여기파장 278 nm, 측정파장 456 nm으로 그리고 유속은 1.0 $m\ell$/min., 주입량은 50 ${\mu}\ell$로 하였다. 확립된 분석조건으로 측정한 ofloxacin, norfloxacin, ciprofloxacin, enrofloxacin 표준품의 표준곡선식에서 모두 상관계수 0.999이상의 양호한 직선성을 보였으며, 첨가한 닭고기의 크로마토그람에서도 각각의 물질별 분리시간대에 방해 피크 없이 양호한 분리도를 나타내었다. 0.05∼0.2 $\mu\textrm{g}$/g 첨가한 시료에서 평균 회수율은 ofloxacin 92.0∼95.4%, norflokacin 84.2∼87.3%, ciprofloxacin 78.3∼82.2%, enrofloxacin 91.3∼95.3%이었으며 변이계수(CV)는 2.7∼9.4%이었다. 4종의 동시분석법의 검출한계 및 정량한계는 각각 ofloxacin 23.5 ppb, 35.3 ppb, norfloxacin 3.4 ppb, 5.1 ppb, ciprofloxacin 3.0 ppb, 4.5 ppb, enrofloxacin 2.5 ppb, 3.8 ppb수준이었다. 2. 인천 지역에서 도축한 닭고기 총 1,523수를 EEC-4-plate법으로 검사한 결과 양성반응을 보인 닭고기는 15수(육계 10, 토종닭 5)였으며, HPLC를 이용한 정밀검사결과 육계 5수에서 ciprofloxacin이 불검출 ∼0.04 ppm, enrofloxacin이 0.01∼0.69 ppm수준으로 검출되었으며, 토종닭 5수에서는 ciprofloxacin이 0.02∼0.12 ppm, enrofloxacin이 0.36∼6.79 ppm수준으로 검출되었다.

유구낭미충(有鉤囊尾蟲) 낭액(囊液)의 아미노산(酸) 및 유리지방산(遊離脂肪酸)의 정량분석(定量分析) (Quantitative Analysis of Cystic Fluid Components in Cysticercus cellulosae)

  • 문준;정명숙;주경환;임한종
    • 농촌의학ㆍ지역보건
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    • 제16권2호
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    • pp.141-153
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    • 1991
  • Free amino acid(FAA), free fatty acid(FFA), and amino acid obtained by hydrolysis of protein components of cystic fluid(CF) of Cysticercus cellulosae in pig and man were analyzed. FFA was analyzed by gas chromatography using Varian model 2700, and flame ionization detector with 6 feet${\times}$1/4inch glass column. Flow rate of $N_2$ was 30 ml/min, $H_2$ was 30 ml/min, air was 350 ml/min respectively and chart speed was 1 cm/min. Amino acid was analyzed by high performance liquid chromatography using Waters model 441, and fluorescence detector at 338nm/425nm with column of amino acid analyzer. Buffer A of mobile phase was pH 3.05 and pH of buffer B was 9.6 respectively. The results obtained were as follows : Seven FFAs containing 12~18 carbons were detected : Saturated fatty acids were lauric acid ($C_{12}$), myristic acid($C_{14}$), palmitic acid($C_{16}$), Stearic acid($C_{18}$). Unsaturated fatty acids were oleic acid($C_{12}^{=1}$), linoleic acid($C_{12}^{=2}$), and one unidentified fatty acid was detected. Generally much more quantity of FFA was determined in CF obtained from pig than that from man. FFA of the largest quantity was palmitic acid; 0.078 mg/ml. Eighteen FAAs were detected and the largest quantity was alanine. Ouantity of alanine was 386 ug/ml in CF from pig 108 ug/ml in CF from man respectively. while histidine in CF from pig was 273 ug/ml, that from man was only 4.3 ug/ml. Eighteen amino acids were identified by hydrolysis of protein in CF from man. But, histidine was not identified in CF from pig. Amino from pig and ug/ml from man.

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신바로 약침의 한약재 확인시험 및 HPLC-DAD를 통한 표준화 연구 (A Study on Standardization of Shinbaro Pharmacopuncture Using Herbal Medicines Identification Test and HPLC-DAD)

  • 이진호;김민정;이재웅;김미령;이인희;김은지
    • Journal of Acupuncture Research
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    • 제32권2호
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    • pp.1-9
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    • 2015
  • Objectives : The present study was an evaluation and standardization of herbal components in order to establish the efficacy and safety of Shinbaro pharmacopuncture. Methods : Among the raw materials of Shinbaro pharmacopuncture, the components Cibotii Rhizoma, Eucommiae Cortex, and Ledebouriellae Radix were assessed through ingredient verification experiments using thin-layer chromatography(TLC) and ultraviolet rays(UV) lamps. In addition, we standardized Acanthopanacis Cortex and Achyranthis Radix through validation using high performance liquid chromatograph-diode array detector(HPLC-DAD). Results : As result appeared a blue-white fluorescence under ultraviolet rays; changed to dark green after adding 1 % ferric chloride solution(due to Cibotii Rhizoma), and presented a yellow-green fluorescence when mixed with an ethyl ether under UV lamps by way of the ethyl ether layer, confirming Eucommiae Cortex. Ledebouriellae Radix was confirmed as dark brown spots at Rf values of 0.56 and 0.71 using TLC. Additionally, Acanthopanacis Cortex and Achyranthis Radix HPLC test results showed that linearity was $R^2{\geq}0.99$, and detection limit and quantitation limit were 0.23 to $1.29{\mu}g/mL$, and 0.71 to $3.90{\mu}g/mL$, respectively. Furthermore, precision and accuracy were confirmed to have relative standard deviation(RSD) values of 0.10 to 1.89 % and 96.19 to 103.72 %, respectively. Shinbaro pharmacopuncture did not have any overlapping or interference from other peaks in detection under the abovementioned analysis conditions. Conclusions : In conclusion, we confirmed that maintenance of Shinbaro pharmacopuncture validity was possible by means of quality control of Cibotii Rhizoma, Eucommiae Cortex, and Ledebouriellae Radix through ingredient identification and Acanthopanacis Cortex and Achyranthis Radix through high performance liquid chromatograph(HPLC) analysis. Further, we hope to contribute to the development strategy of herbal industry acupuncture.

HPLC를 이용한 사료 중 Deoxynivalenol, Zearalenone의 분석과 오염도 조사 (Analysis and Survey for Contamination of Deoxynivalenol and Zearalenone in Feed by High Performance Liquid Chromatography)

  • 김동호;최규일;홍경숙;김현정;송영진;강승훈;장한섭;조현정;한계수
    • 한국식품위생안전성학회지
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    • 제26권3호
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    • pp.214-221
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    • 2011
  • 2010년 유통사료 113점에 대하여 곰팡이독소 오염도 조사를 실시하였다. 면역친화컬럼(IAC)을 이용하여 각각 정제하였으며, HPLC/DAD와 FLD를 연결하여 동시분석하였다. DON은 200과 1,000 ${\mu}g/kg$수준에서 각각 95.40과 88.76%의 회수율과 4.03과 1.40%의 상대표준편차(%RSD)를 나타내었다. ZEN은 100과 500 ${\mu}g/kg$ 수준에서 각각 87.09과 98.40%의 회수율과 9.01과 2.81%의 상대표준편차(%RSD)를 나타내었다. 배합사료인 닭사료, 돼지사료, 소사료에서 DON과 ZEN이 각각 372.1, 324.0, 990.9 ${\mu}g/kg$와 76.1, 43.7, 196.2 ${\mu}g/kg$의 평균오염도를 보여 2009년도 조사결과보다 높은 오염수준을 나타내었다. 옥수수, 단백피, 주정박, 옥수수배아박, 옥수수글루텐에서는 DON과 ZEN이 각각 224.6, 3150.4, 721.5, 37.8, 207.3 ${\mu}g/kg$와 77.8, 308.5, 163.1, 116.9, 510.8 ${\mu}g/kg$로 나타남에 따라 역시 배합사료에 곰팡이독소를 오염시키는 주 원인물질로 확인되었다.

RP-HPLC 에 의한 에폭시 통조림관 음료 중 비스페놀류의 분석을 위한 시료의 전처리 (Sample Preparation for Quantitative Determination of Bisphenols in Canned Beverages Coated with Epoxy by RP-HPLC)

  • 강경모;임흥렬;신효선
    • 한국식품과학회지
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    • 제32권5호
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    • pp.1029-1034
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    • 2000
  • 에폭시 수지로 내면 코팅된 통조림의 각종 음료중 비스페놀류(BPF, BPA, BFDGE, BADGE)의 함유량을 형광검출기의 역상 HPLC와 GC/MS에 의해 분석할 때 시료의 처리 방법에 대하여 연구하였다. 음료에 비스페놀류의 표준액을 각각 10, 5, 1 ${\mu}g/L$ 첨가한 후 음료의 종류에 따라 고상추출, 액상추출 및 카트리지 정제 등의 전처리 과정을 통하여 분석한 비스페놀류의 회수율을 측정하였다. 음료에 첨가한 비스페놀 중 BPA와 BADGE는 모든 음료에서 분리, 정량이 가능하였다. 커피, 식혜, 과즙음료에서 BPA의 회수율은 고상추출보다 액상추출이 우수하였으며, diethyl ether에 의한 액상추출이 methylene chloride보다 우수하였다. 탄산음료와 다류에서 BPA의 회수율은 액상추출보다 고상추출이 우수하였다. BADGE의 회수율은 전처리 방법에 관계없이 모든 음료에서 BPA보다 낮았다. 시판되는 통조림 음료 18종에 대하여 최적 전처리 방법으로 처리한 후 비스페놀류의 함유량을 측정한 결과 BPA는 커피, 콜라, 홍차 식혜, 과일쥬스에서 각각 $1.3{\sim}11.6{\mu}g/L,\;0.5{\sim}0.9{\mu}g/L,\;1.0{\sim}1.3{\mu}g/L,\;2.4{\sim}7.9{\mu}g/L,\;3.0{\sim}3.4{\mu}g/L$였으며, 맥주는 모두 검출한계($0.2{\mu}g/L$)이하였다.

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알칼리분해를 이용한 어류 중 다환방향족탄화수소의 전처리방법 (Pretreatment of Fish for the determination of polycyclic aromatic hydrocarbons using alkali digestion)

  • 허수정;이효민;채영주;유은아
    • 분석과학
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    • 제18권5호
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    • pp.403-409
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    • 2005
  • 최근 내분비계장애물질로 알려진 PAHs 화합물 중 하나인 벤조피렌은 대표적인 PAHs 화합물로 음식을 조리, 가공할 때 식품의 주성분인 탄수화물, 단백질, 지방 등이 분해되어 생성되는 열분해 산물이며 토양, 공기, 물, 식품 등 전 환경매체에서 검출되고 있다. 본 연구에서는 PAHs[benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene, indeno(1,2,3-c,d)pyrene]에 대하여 어류 중 지방의 알칼리 분해시간에 따른 분해효율, 추출 용매에 따른 추출효율, 정제컬럼의 용출량에 따른 정제효율 등을 비교 실험하여 알칼리분해를 이용한 어류 중 PAHs의 전처리방법을 확립하고자 하였다. 균질화된 시료를 알칼리 분해하여 n-hexane으로 추출하고 증류수로 세척한 후 Sep-Pak florisil cartridge로 정제하여 HPLC/FLD(고속액체크로마토그래피/형광검출기) 로 동시 정량 분석하였으며 각각의 PAHs에 대한 회수율은 약 90~106% 수준이었다.

Simultaneous Fluorimetric Determination of On-line Preconcentrated HANs, DCAD and TCAD by Using RPLC with a Postcolumn Derivatization System

  • Jung, Sung-Woon;Choi, Yong-Wook
    • Bulletin of the Korean Chemical Society
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    • 제34권6호
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    • pp.1783-1790
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    • 2013
  • A simultaneous analytical method has been developed for the fluorimetric determination of haloacetonitriles (HANs) [dichloroacetonitrile (DCAN), trichloroacetonitrile (TCAN), dibromoacetonitrile (DBAN), haloacetamides [dichloroacetamide (DCAD), and trichloroacetamde (TCAD)] in drinking water by using the combined on-line perconcentration/reversed phase liquid chromatography (RPLC)-postcolumn detection system. This on-line perconcentration system was achieved by employing a precolumn packed with a commercial solid phase extraction (SPE) sorbent for the enrichment and purification of the target analytes. The haloacetonitriles and haloacetamides were separated on CN analytical column in a 7.5% methanol-0.02 M phosphate buffered mobile phase at pH 3. The column effluents were reacted with postcolumn reagents of ophthaldialdehyde (OPA) and sulfite ion at pH 11.5, to produce a highly fluorescent isoindole fluorophore, which were measured with a fluorescence detector. Under the optimized conditions for RPLC and the postcolumn derivatization system all of the coefficient of determination of the standard calibration curves for the target analytes were over 0.99 and had a linear range from 5 to 100 ${\mu}g/L$. The detection limits showed 1.6 ${\mu}g/L$ for DCAD, 0.1 ${\mu}g/L$ for TCAD, 0.6 ${\mu}g/L$ for DCAN, 1.6 ${\mu}g/L$ for TCAN and 1 ${\mu}g/L$ for DBAN, and the recoveries were ranged from 64 to 99% except for DCAD with precisions less than 4.9% in distilled water, and from 72(${\pm}4%$) to 116%(${\pm}2%$) in tap water.

서울시 지하상가 공기중 다환방향족 탄화수소의 농도조사에 관한 연구 (Measurements of Polycyclic Aromatic Hydrocarbons(PAHs) Concentration in Air of the Seoul Underground Shopping Stores)

  • 전준민;김윤신
    • 한국대기환경학회지
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    • 제9권1호
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    • pp.81-92
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    • 1993
  • A purpose of this study was carried out to investigate the concentrations of four elements of PAHs(Polycyclic Aromatic Hydrocarbons) in suspended particulate matters of underground shopping stores in Seoul city. The particulate matters were collected at five underground shopping stores(Yongdungpo, Myongdong, Ulchiro, Express Terminal, Chamshil) in the Seoul area during February-October, 1992. Samples were collected using cascade impactor of low volumn air sampler and were analysed using High Performance Liquid Chromatography(HPLC) with fluorescence detector. Calibration on HPLC analyse is nearly accord with retention time between the standard solution and the samples. Analysed results obtained favorable analysing recovery rate of 97.3% and coefficient of variation of 1.60%. Mean concentrations of suspended particulate matters in five underground shopping stores wre 216.3 g/$m^3$ and observed higher at fine particles(117.2 g/$m^3$) which is respirable particulates than coarse particles(99.2 g/$m^3$). Concentrations of four species PAH were determined with anthracene of 16.8ng/$m^3$, fluoranthene of 72.3ng/$m^3$, benzo(a)pyrene of 0.54ng/$m^3$, and benzo(k)fluoranthene of 0.29ng/$m^3$, respectively. Fluoranthene levels were significantly higher than those levels in other components. PAHs concen-tration at shopping areas showed 21.3ng/$m^3$ in Yongdungpo, 35.1ng/$m^3$ in Myongdong, 23.4ng/$m^3$ in Ulchiro, 11.1ng/$m^3$ in Express Terminal, and 21.4ng/$m^3$ in Chamshil, respectively. Particularly, benzo(a)pyrene and benzo(k)-fluoranthene were detected over 83 percentage in fine particles, while fluoranthene wre highly detected in coarse particles. Also, higher concentrations of benzo(a)pyrene, benzo(k)fluoranthene were found in winter while levels of anthracene and fluoranthene were found higher in summer than other seasons.

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