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

검색결과 71건 처리시간 0.027초

UV-Vis 분광분석에 의한 전기변압기 내 절연지 열화도 측정 (Application of UV-Vis Spectroscopic Analysis for Transformer Insulating Paper Degradation)

  • 공호성;한흥구
    • Tribology and Lubricants
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    • 제35권3호
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    • pp.151-157
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    • 2019
  • Insulated oil degradation produces charged by-products, such as acids and hydro-peroxides, which tend to reduce the insulating properties of the oil. In this study, UV-vis spectroscopy measurement technology is developed and experimentally compared with other measurement methods, such as the titration method and IR spectroscopy, to validate its ability to monitor the degradation of electrical insulating paper. The degradation characteristics of the insulating paper are appropriately represented through various types of measurement methods, such as the Tan (delta) method, $CO_2$ gas production measurement, the titration method, and IR spectroscopy. The results are demonstrated to be well comparable to a change in the fluorescence emission ratio (FER), which is defined as the shift in fluorescence intensity in the measured wavelength range, and also to the chromatic ratio, which is defined as a color shift to longer wavelength ranges. The results also show that, by using UV-vis spectroscopy, it is possible to detect the degradation of the insulating paper. This study suggests that UV-vis spectroscopy can be applied as an alternative to high-performance liquid chromatography, which is the internationally recognized measurement technology for cellulose paper degradation. The FER detector is also verified to be useful as an effective condition-monitoring device for power transformers.

경기남부지역 원유중의 설파제 잔류조사 (Determination of Sulfonamide Residues in Raw Milk from southern Kyeonggi Area)

  • 김창수;이성권;고태오;고신일
    • 한국동물위생학회지
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    • 제19권1호
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    • pp.39-45
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    • 1996
  • Sulfonamides are widely used to treat mastitis of cattle in field. The study was carried out to analyze sulfonamid residues In raw milk from south Kyeonggi area. The milk sample was deproteinated with acetone and defatted with hexane. The residual sulfonamides were extracted with ethylacetate, concentrated under vaccum, reconstituted with the acetate buffer-methanol mixture, reacted with fluorescamine, and then analyzed by HPLC-fluorescence detector(EX. 39nm, Em. 495nm) with methanol : acetate buffer system(3/2, v /v) as a mobile phase. The results analyzed by Thin layer chromatography and High performance liquid chromatography were summarized as follows. 1. A total of 24 cases out of 478 raw milk samples(5.0%) collected during April and May showed positive reaction to sulfonamide residues. Among 24 positive reactors, 9 cases were positive to sulfanilamides(32.1%), 8 cases were positive to sulfathiazoles(28.6%) and 5 cases were positive to sulfamonomthoxines (7.9%) , respectively. 2. During July and August, 31 cases out of 464 raw milk samples(6.7%) showed positive re action to sulfonamide residues. Among them S cases were positive to sulfanilamides, 5 cases sulfathiazoles and 5 cases sulfamonomethoxines(16.1%), respectively.

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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.

Simplified HPLC Method for the Determination of Prazosin in Human Plasma and Its Application to Single-dose Pharmacokinetics

  • Gwak, Hye-Sun;Chun, In-Koo
    • Biomolecules & Therapeutics
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    • 제13권2호
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    • pp.90-94
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    • 2005
  • Prazosin hydrochloride is an antihypertensive drug with selective ${\alpha}_1$-adrenoreceptor blocking effects. A simple high performance liquid chromatographic method has been developed and validated for the quantitative determination of prazosin in human plasma. A reversed-phase C18 column was used for the separation of prazosin and terazosin (internal standard) with a mobile phase composed of water, acetonitrile and triethylamine(75:25:0.1, V/V;pH5.0) at a flow rate of 1.5 ml/min. the fluorescence detector was set at excitation and emissionwavelengths of 250 and 370 nm, respectively. Intra-and inter-day precision and accuracy were acceptable for all quality control samples including the lower limit of quantification of 0.5 ng/ml. Good recovery (>80%) was seen in plasma. Prazosin was stable in human plasma under various storage conditions. This method was used successfully for a pharmacokinetic study in plasma after oral administration of a single 2-mg dose as prazosin base to 16 healthy volunteers. The maximum plasma concentration of prazosin was 23.1 ${\pm}$ 16.5 ng/ml at 2.1 h, and the mean area under the curve and elimination half-life were calculated to be 108.4 ${\pm}$ 74.2 ng ${\cdot}$hr/ml and 2.5 ${\pm}$ 0.6 h, respectively.

Simplified HPLC Method for the Determination of Mirtazapine in Human Plasma and Its Application to Single-dose Pharmacokinetics

  • Gwak Hye-Sun;Lee Na-Young;Chun In-Koo
    • Biomolecules & Therapeutics
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    • 제14권1호
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    • pp.40-44
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    • 2006
  • Mirtazapine is an antidepressant agent with dual action on both the noradrenergic and serotonergic neurotransmitter systems. A simple high performance liquid chromatographic method has been developed and validated for the quantitative determination of mirtazapine in human plasma. A reversed-phase Cl8 column was used for the determination of mirtazapine with a mobile phase composed of 0.01M ammonium acetate solution (pH 4.2) and acetonitrile (75:25, v/v%) at a flow rate of 1.2 mL/min. Terazosin hydrochloride was used as an internal standard. The fluorescence detector was set at excitation and emission wavelengths of 290 and 350 nm, respectively. Intra- and inter-day precision and accuracy were acceptable for all quality control samples including the lower limit of quantification of 3 ng/mL. Mirtazapine was stable in human plasma under various storage conditions. This method was used successfully for a pharmacokinetic study using plasma samples after oral administration of a single 30 mg dose as mirtazapine base to 8 healthy volunteers. The maximum plasma concentration of mirtazapine was $64.1{\pm}28.0ng/mL$ at 1.8 h, and the area under the curve and elimination half-life were calculated to be $674.1{\pm}218.5ng\;h/mL\;and\;23.4{\pm}3.8h$, respectively.

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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만성신부전증환자에서 HPLC/FLD를 이용한 혈장 Homocysteine의 측정 (Measurement of Total Plasma Homocysteine in Patients with Chronic Renal Failure Using HPLC/FLD)

  • Kyung-Ok Lee;Bo-Kyung Kang;Hyung-Jin Roh;Kwang-Suk Ryoo;Jeong-Yeon Yoo;Man-Jeong Paik;Kang-Hyeob Lee
    • 대한의생명과학회지
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    • 제3권1호
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    • pp.29-35
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    • 1997
  • 본 연구에서는 한국인 만성신부전증 환자에서 심혈관계 질환의 조기진단을 위한 생화학적 표지 자로서 homocysteine의 임상적 유용성을 검토하기 위하여, 만성신부전증 환자와 건강인에서 HPLC/FLD (high performance liquid chromatography/fluorescence detector)를 이 용하여 혈장 homocysteine 농도를 측정하고 그 결과를 비교하였다. 본 실험방법의 회수율은 98.6$\pm$5.8%를 나타내었으며, 0.2 nmol/L 보다 낮은 농도까지 측정이 가능하였고, 2~50 nmol/ml까지 직선성이 성립하였다 (correlation coefficient =0.9997). 한국인 중 건강한 정상인 (20명)과 만성신부전증 환자 (90명)에서 혈장 homocysteine은 각각 6.81$\pm$1.54 nmol/ml과 27.28$\pm$14.94 nmol/ml이었으며 , 환자군에서는 정상인군에 비하여 약 4배정도 높은 수치를 나타내었다 (p<0.05).본 실험의 결과로 볼 때 HPLC/FLD를 이용한 homocysteine 측정은 예민도와 재현성이 높아 routine 실험실 방법으로 유용성이 높을 것으로 생각되며, 또한 혈장 homocysteine의 측정은 만성신부전증 환자의 주요한 사망원인이 되는 폐쇄성 동맥질 환을 조기에 진단하거나, 혹은 homocysteine 농도를 저하시키는 치료를 실시 한 후 치료효과를 판단하기 위한 생화학적 marker로 활용될 수 있을 것으로 기대된다.

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호소수를 원수로 사용하는 정수장의 소독부산물 생성 특성 및 제어 방안 (Formation Characteristics and Control of Disinfection Byproducts in a Drinking Water Treatment Plant Using Lake Water)

  • 이기창;제갈봉창;최일환;이원태
    • 대한환경공학회지
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    • 제37권5호
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    • pp.269-276
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    • 2015
  • 본 연구는 경상북도 지역에서 호소수를 원수로 사용하는 한 정수장의 원수 및 공정별 처리수의 자연유기물질(NOM) 및 소독부산물(DBPs) 생성특성을 조사하고 정수공정내 DBPs 제어방안을 제시하였다. Fluorescence excitation-emission matrix (FEEM) 분석결과 원수의 NOM은 토양과 미생물의 복합기원에 의한 것으로 밝혀졌다. NOM의 분자량크기 및 분획제거 특성은 liquid chromatography-organic carbon detector (LC-OCD)를 이용하여 분석하였다. 대체로 휴믹물질과 저분자량 유기물질 분획이 많았고, 고분자량물질은 저분자량물질보다 응집 침전공정에서 제거가 용이한 것으로 나타났다. 전염소주입 후 정수공정별로 진행될수록 반응시간이 길어져 DBPs 농도가 증가하였으며 생성된 DBPs는 일반적인 정수처리로 제거되지 않았다. THMs은 chloroform이 74%로 주종을 이루었으며 bromodichloromethane (22%)와 dibromochloromethane (4%)도 발생했다. HAAs는 dichloroacetic acid (50%)와 trichloroacetic acid (48%)가 주종을 이루었고 dibromoacetic acid (2%) 등 브롬계열은 농도가 낮거나 발생되지 않았다. HANs은 dichloroacetonitrile (60%), bromochloroacetonitrile (30%), dibromoacetonitrile (10%)이 발생되었다. 실험기간 동안 해당 정수장에서 DBPs 발생은 용존유기물농도와 수온보다 전염소주입농도에 큰 영향을 받은 것으로 나타났고, 염소주입농도의 조절로 DBPs 생성농도를 이전에 비해 16~44% 감소시킬 수 있었다.

수산물 조리 식품에 함유된 수용성 비타민 함량 (Water-Soluble Vitamins Contents in Seafood-Based Dishes)

  • 김나은;김영화
    • 한국식품영양학회지
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    • 제33권4호
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    • pp.390-398
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    • 2020
  • The purpose of this study was to determine the contents of water-soluble vitamins B1 (thiamine), B2 (riboflavin), B3 (niacin) and B12 (cyanocobalamin) in seafood-based dishes by using the high-performance liquid chromatography with the ultra violet and fluorescence detector. The vitamin B1, B2, B3 and B12 contents were analyzed in 29 seafood-based dishes. The method validation was performed on the method to determine the linearity, accuracy, limits of quantification, limits of detection and precision for vitamin B1, B2, B3 and B12. An excellent linearity range (R2=0.999~1.000) in the calibration curve for the water-soluble vitamins was observed. All analytical methods for the water-soluble vitamins showed the acceptable accuracy (89.4~119.7% recovery) and the precision (0.6~4.8% repeatability and 1.0~4.2% reproducibility). The highest content of vitamin B1 was 2.646 mg/100 g in the kkongchi-jorim, and the highest contents of vitamin B2, B3 and B12 were 0.370 mg/100 g, 10.971 mg/100 g, and 17.193 ㎍/100 g, respectively, in the kkongchi-gui. Our results provide reliable data on the contents of the water-soluble vitamins of seafood-based dishes in Korea.