• 제목/요약/키워드: fluorescence detector

검색결과 185건 처리시간 0.029초

나부메톤 정의 생물학적 동등성 평가 (Bioequivalence of Nabumetone Tablets)

  • 이윤석;박은석;지상철
    • Journal of Pharmaceutical Investigation
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    • 제27권3호
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    • pp.207-212
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    • 1997
  • The bioequivalence of two nabumetone tablets was evaluated in 16 normal male volunteers $(age\;21{\sim}30\;yrs)$ following oral administration. Test product was 'Nacton tablet' made by Jin Yang Pharmaceutical Co. and reference product was 'Unimeton tablet' made by Dong Kwang Pharmaceutical Co.. After one tablet containing 500 mg of nabumetone was administered, blood was taken at predetermined time intervals and the concentration of 6-methoxy-2-naphthylacetic acid, active metabolite of nabumetone, in plasma was determined with an HPLC method using fluorescence detector. AUC, $C_{max}$ and $T_{max}$ were calculated and statistically analyzed for the bioequivalence of the two products. The results showed that the differences in AUC, $C_{max}$ and $T_{max}$ between two products were 3.66%, 6.87% and 1.85%, respectively. The powers$(1-{\beta})$ for AUC, $C_{max}$ and $T_{max}$ were 91.4%, 88.9% and 81.1%, respectively. Detectable differences$({\Delta})$ and confidence intervals were all less than 20%. All of these parameters met the criteria of FDA for bioequivalence, indicating that "Nacton tablet" is bioequivalent to 'Unimeton tablet'.

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An integrated DNA barcode assay microdevice for rapid, highly sensitive and multiplex pathogen detection at the single-cell level

  • Jung, Jae Hwan;Cho, Min Kyung;Chung, So Yi;Seo, Tae Seok
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제45회 하계 정기학술대회 초록집
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    • pp.276-276
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    • 2013
  • Here we report an integrated microdevice consisting of an efficient passive mixer, a magnetic separation chamber, and a capillary electrophoretic microchannel in which DNA barcode assay, target pathogen separation, and barcode DNA capillary electrophoretic analysis were performed sequentially within 30 min for multiplex pathogen detection at the single-cell level. The intestine-shaped serpentine 3D micromixer provides a high mixing rate to generate magnetic particle-pathogenic bacteria-DNA barcode labelled AuNP complexes quantitatively. After magnetic separation and purification of those complexes, the barcode DNA strands were released and analyzed by the microfluidic capillary electrophoresis within 5 min. The size of the barcode DNA strand was controlled depending on the target bacteria (Staphylococcus aureus, Escherichia coli O157:H7, and Salmonella typhimurium), and the different elution time of the barcode DNA peak in the electropherogram allows us to recognize the target pathogen with ease in the monoplex as well as in the multiplex analysis. In addition, the quantity of the DNA barcode strand (~104) per AuNP is enough to be observed in the laser-induced confocal fluorescence detector, thereby making single-cell analysis possible. This novel integrated microdevice enables us to perform rapid, sensitive, and multiplex pathogen detection with sample-in-answer-out capability to be applied for biosafety testing, environmental screening, and clinical trials.

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HPLC법에 의한 1,2-디아미노-4,5-메틸렌디옥시벤젠을 형광유도체화제로 한 혈청 및 뇨 중의 ${\alpha}$-케토산의 분석 (Determination of ${\alpha}-Keto$ Acids in Serum and Urine Using 1,2-Diamino-4,5-methylendioxybenzene as a Fluorescent Derivatizating Agent by High Performance Liquid Chromatography)

  • 옥치완;김대기;박송자;박종세
    • 약학회지
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    • 제36권4호
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    • pp.370-378
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    • 1992
  • A simple and sensitive high performance liquid chromatographic method to quantitate ${\alpha}-keto$ acids in serum and urine was investigated. ${\alpha}-Keto$ acids react with 1,2-diamino-4,5-methylenedioxybenzene (DMB) in the presence of 2-mercapto-ethanol and sodium hydrogen sulfite to form highly fluorescent derivatives, substituted 6,7-methylenedioxyquinoxalinol. The derivatization procedure was performed in water bath at $100^{\circ}C$, and completed within 50 min. By the use of a reversed-phase column and multi-step gradient with two solvents, a mixture containing twelve of these derivatives were efficiently resolved within 35 minutes. The optimal wavelengh of the fluorescence detector are ${\lambda}_{ex}=364\;nm$ and ${\lambda}_{em}=445\;nm$. The quantitation of the individual ${\alpha}-Keto$ acids was reproducible with relative standard deviation of $3.0{\sim}7.9%$ and had a detection limits of $10{\sim}60$ fmol, except for p-hydroxyphenylpyruvic acid (960 fmol).

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Pharmacokinetic Behavior and Tissue Distribution of Verapamil and Its Enantiomers in Rats by HPLC

  • He, Langchong;Wang, Sicen
    • Archives of Pharmacal Research
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    • 제26권9호
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    • pp.763-767
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    • 2003
  • The differences in pharmacokinetic behavior and tissue distribution of verapamil and its enantiomers were investigated in rats. In high-performance liquid chromatographic method, an achiral ODS column (150 mm $\times$ 4.6 mm i.d.) with the mobile phase consisting of methanol-water (73:30, v/v) was used for the determination of the concentration for racemic verapamil, and a Chiralcel OJ column (250 mm$\times$4.6 mm i.d.) with the mixture of n-haxane-ethanol-triethylamine (85:15:0.2, v/v/v) as mobile phase was used to determine the concentrations of verapamil enantiomers. A fluorescence detector in the analytical system was set at excitation and emission wavelengths of 275 nm and 315 nm. The differences between enantiomers were apparent in the pharmacokinetics in rats. The area under the concentration-time curve (AUC) of S-(-) verapamil was higher than that of R-(+) verapamil. The half-distribution time ($T_{1/2(\alpha)}$) of S-(-) verapamil which distributing to tissue from blood was shorter than that of R-(+) verapamil, but the elimination half-time ($T_{1/2(\beta)}$) was longer in rat following oral administration of racemic verapamil. At 1.3 h after oral administration of racemic verapamil, however, there were no significant differences between enantiomers for the distributions in major tissues such as heart, cerebrum, cerebellum, liver, spleen and kidney.

Determination of L-Carnitine in Infant Powdered Milk Samples after Derivatization

  • Park, Jung Min;Koh, Jong Ho;Kim, Jin Man
    • 한국축산식품학회지
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    • 제41권4호
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    • pp.731-738
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    • 2021
  • Herein, a novel analytical method using a high-performance liquid chromatography-fluorescence detector (HPLC/FLD) is developed for rapidly measuring an L-carnitine ester derivative in infant powdered milk. In this study, solid-phase extraction cartridges filled with derivatized methanol and distilled water were used to effectively separate L-carnitine. Protein precipitation pretreatment was carried out to remove the protein and recover the analyte extract with a high recovery (97.16%-106.56%), following which carnitine in the formula was derivatized to its ester form. Precolumn derivation with 1-aminoanthracene (1AA) was carried out in a phosphate buffer using 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) as the catalyst. Method validation was performed following the AOAC guidelines. The calibration curves were linear in the L-carnitine concentration range of 0.1-2.5 mg/L. The lower limit of quantitation and limit of detection of L-carnitine were 0.076 and 0.024 mg/L, respectively. The intra- and interday precision and recovery results were within the allowable limits. The results showed that our method helped reduce the sample preparation time. It also afforded higher resolution and better reproducibility than those obtained by traditional methods. Our method is suitable for detecting the quantity of L-carnitine in infant powdered milk containing a large amount of protein or starch.

인천지역 유통 과일 중 잔류농약 모니터링 및 위해성 평가 (Monitoring of Pesticide Residues and Risk Assessment in Some Fruits on the Market in Incheon, Korea)

  • 정세진;김혜영;김지형;염미숙;조중희;이수연
    • 한국환경농학회지
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    • 제33권2호
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    • pp.111-120
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    • 2014
  • 인천시내에 유통되는 오렌지, 키위 등 215건의 과일에 대하여 분석대상 농약 259종에 대한 잔류농약 모니터링을 실시하였다. 전체 수거 과일의 56.3%에서 기준이내 농약이 검출되었으며, 이중 수입과일은 60.8%, 국내산 과일은 45.1%의 검출률을 나타내었으나 농약잔류허용기준을 초과한 품목은 없었다. 그 중 감귤류의 농약 검출률은 83.9%로 상당히 높은 수준으로 나타났다. 농약성분별 검출빈도는 carbendazim(13.1%), imazalil(11.7%), thiabendazole(10.7%), fludioxonil(9.8%) 순으로, 검출된 농약의 위해성 평가결과 해당 농산물섭취에 따른 인체 유입 농약의 일일섭취추정량 ADI%는 0.00011~0.98795% 수준으로 위해성은 낮은 것으로 추정된다. 또한, 감귤류와 같은 과피를 제거 하고 섭취하는 과일은 과피 제거로 91.6%의 잔류농약 경감 효과를 나타내었으며, 세척 후 섭취하는 형태인 포도나 체리 등은 수돗물 침지 후 세척법에 의해서 평균 43.1%의 잔류농약 감소를 보여, 과일섭취에 따른 위해성 역시 상당부분 감소할 것으로 보인다.

경기도내 유통 수입과실류의 잔류농약 실태조사 (A survey on pesticide residues of imported fruits circulated in Gyeonggido)

  • 조윤식;강정복;김양희;정진아;허정원;이소현;임영식;배호정;강흥규;이정희;정은숙;이병훈;박용복;이정복
    • 농약과학회지
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    • 제16권3호
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    • pp.195-201
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    • 2012
  • 본 연구는 경기도에서 유통 중인 수입과실류에 대한 잔류농약 분석을 수행하였다. 총 22품목 124건의 시료를 구입하여 GC/NPD-ECD, TOF/MS, UPLC/PDA 및 HPLC/FLD, LC/MS/MS를 이용하여 218종 잔류농약을 동시 다성분 분석법으로 분석한 결과 18건의 과실에서 잔류농약이 0.003~0.3 mg/kg 범위로 검출되었으나 기준초과 시료는 없었다. 과실의 부위별 특성에 따른 잔류농약정도를 알아보기 위해 농약이 검출된 과실류 중 14건에 대하여 분리 실험을 실시하였으며, 그 결과 과피 14건에서 0.03~1.5 mg/kg, 과육의 경우 2건에서 검출한계 미만으로 나타났다. 실험결과 모두 잔류농약허용기준 이내에서 검출되어 정상적인 방법으로 섭취할 경우 위해도는 매우 낮은 수준이었다. 그러나 미량이라도 장기간 섭취시 인체에 유해할 수 있으며, 검출빈도가 높은 성분들이 검출되므로 수입과실에 대한 지속적이고 체계적인 모니터링이 필요하겠다.

서울시 유통 건조농산물 중의 농약잔류 실태 연구 (A Study of Current Status on Pesticide Residues in Commercial Dried Agricultural Products)

  • 김복순;박성규;김미선;조태희;한창호;조한빈;최병현;김성단
    • 한국식품과학회지
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    • 제39권2호
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    • pp.114-121
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    • 2007
  • 서울지역에 유통되고 있는 국내산 및 수입산 건조농산물 58건을 대상으로 다성분 동시분석방법에 따라 GC-NPD, $GC-{\mu}ECD$, HPLC-UV와 HPLC-FLD로 분석가능한 총 253종의 농약잔류량을 분석한 후 GC-MSD로 확인한 결과 총 14건의 건조농산물에서 잔류농약이 검출되어 24.1%의 검출률을 나타내었고, 이 중 건조 채소류의 검출률은 25.5%였다. 품목별 잔류농약의 검출률은 건조과채류, 건조엽채류, 건조엽경채류 순으로 높았으며, 특히 건조 과채류 중 건조고추의 잔류농약 분포가 다양하고 검출빈도가 상당히 높았다. 건조 농산물의 기준에 없는 12종의 잔류농약이 검출되었으며, 합성피레스로이드계, 유기염소계, 유기인계 순으로 검출빈도가 높았고, 특히 합성피레스로이드계 중 cypermethrin의 검출 횟수가 가장 많았다. 또한 대상목적에 따라 분류하면, 살충제, 살균제, 제초제, 살선충제 순서로 검출건수가 많았다. 산지별로 보면, 국내산, 중국산 ,북한산, 미국산, 베트남산의 순서로 잔류농약의 검출건수가 많았으며, 국내산은 과채류에서 수입산은 엽경채류에서 잔류농약의 검출빈도가 높았다.

환경성 PAHs 노출과 생체지표 연구 (Urinary PAH Metabolites as Biomarkers of Environmental PAHs Exposure)

  • 이경호;이충민;조수헌;권호장;강대희
    • Toxicological Research
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    • 제23권1호
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    • pp.39-46
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    • 2007
  • The aim of the study was to see if there is any differences in urinary 1-hydroxypyrene glucuronide (1-OHPG) and 2-naphthol levels in children ($8{\sim}14$ years old) and their mothers ($30{\sim}46$ years old) living three cities in South Korea (Seoul, Incheon and Pohang) and three in China (Changchun, Datong and Kunming), where the levels of air pollution varies. The factors related with urinary biomarkers levels were also evaluated. The study subjects consisted of 118 Korean (60 children and 58 their mothers) and 120 Chinese (60 children and 60 their mothers). Urinary 1-OHPG was measured by synchronous fluorescence spectroscopy after immuno-affinity purification using monoclonal antibody 8E11 and urinary 2-naphthol concentrations were determined by HPLC with fluorescence detector. Information on recent consumption of diet containing high PAHs, environmental tobacco smoke (ETS), type of cooking and heating fuels, and other life-style characteristics were collected by self-administered questionnaire. The arithmetic mean of urinary 1-OHPG levels (n = 120, $mean{\pm}SD$, $6.77{\pm}7.96{\mu}mol/mol$ creatinine) in Chinese were 10 fold higher than those in Korean (n = 118, $0.62{\pm}0.61{\mu}mol/mol$ creatinine) (P < 0.01). Urinary 2-naphthol levels in Chinese (n = 119, $59.50{\pm}82.29{\mu}g/g$ creatinine) were significantly higher than those in Korean (n = 117, $25.09{\pm}46.56{\mu}g/g$ creatinine) (P < 0.01). Urinary 1-OHPG and 2-naphthol levels were significantly higher in children living the polluted cities in China (Datong and Chanchun, respectively). Multiple linear regression analysis indicated that living in factory area (vs. residential area) and use of coal stove as heating fuel were significant predictors for urinary 1-OHPG (overall model $R^2$= 0.46, n = 204). And ETS was predictor for urinary 2-naphthol levels in Korean ($R^2$ = 0.36, n = 46). These results indicated that urinary 1-OHPG and 2-naphthol levels were related with different ambient particulate air pollution, type of heating fuels and ETS.

HPLC-FLD 및 LC-MS/MS에 의한 식품 중 총아플라톡신 오염실태 조사 (A Survey of Total Aflatoxins in Food Using High Performance Liquid Chromatography-Fluorescence Detector (HPLC-FLD) and Liquid Chromatography Tandem Mass Spectrometry(LC-MS/MS))

  • 장미란;이창희;조성혜;박준식;권은영;이은진;김소희;김대병
    • 한국식품과학회지
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    • 제39권5호
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    • pp.488-493
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    • 2007
  • 국내유통중인 곡류, 견과류 및 그 가공품 총 25품목, 393건의 시료에 대해 immunoaffinity column 정제방법을 이용하여 총아플라톡신 오염실태를 조사하였으며, 그 결과 곡류 및 곡류가공품 6건, 견과류 및 견과류 가공품 37건에서 아플라톡신 오염이 확인되었으며 오염수준은 아플라톡신 $B_1$으로서 $0.04-2.65{\mu}g/kg$, 총아플라톡신으로서 $0.04-5.51{\mu}g/kg$ 범위로 나타났다. Immunoaffinity column 정제를 거쳐 HPLC-FLD로 분석한 결과 아플라톡신이 검출된 시료에 대해서 LC-MS/MS로 확인하였으며, 그 결과 모두 아플라톡신으로 확인되었다. 본 연구결과에서 나타난 곡류 및 견과류에 대한 아플라톡신 검출빈도 및 오염수준은 국내, 외 연구 결과와 유사하거나 비교적 낮게 나타났으며 국내 아플라톡신 기준 및 미국, CODEX에서 설정된 기준규격 이하로 검출되었다.