• Title/Summary/Keyword: peak detector

검색결과 324건 처리시간 0.025초

새로운 유도체 합성법에 의한 토양침투수중 2,4-D, dicamba 및 mecoprop의 동시 분석법에 관한 연구 (New Esterification Method for the Simulataneous Analysis of 2,4-D, Dicamba and Mecoprop in Soil Leachates by GC/MS and GC/ ECD)

  • 홍무기;이희덕;박건상
    • 한국환경농학회지
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    • 제14권1호
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    • pp.45-54
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    • 1995
  • esters of the acid analytes were synthesized using $H_2SO_4$ as the catalyst. Efficiency of derivatization and instrumental molecular-response were compared with herbicides methylated with $BF_3-methanol$(14% W/V), $H_2SO_4-methanol$(33% V/V), and diazomethane. The molecular integrity of TFE-2,4-D, TFE-dicamba, and TFE-mecoprop, in the mixture, was confirmed by the GC/MSD method. The TFE-Esterification efficiency was maximized by adjusting the volume of $H_2SO_4$ the reaction time, and temperature. Optimal efficiency for the herbicide mixture was obtained by adding 1 ml of $H_2SO_4$ and 1 ml of TFE to the dried sample and allowing the reaction to proceed at $22^{\circ}C$ for 8 hr or using 0.5 ml $H_2SO_4$ and 1 ml of TFE at $60^{\circ}C$. For 120 min increasing the temperature and decreasing the reaction time were required for maximum esterification efficiency. The sensitivity of the GC/ECD to the TFE esters was about $2{\sim}20$ times greater than that to the methyl ester derivatives. The herbicides were extracted and esterified to TFE derivatives simultaneously from soil leachates previously spiked with the analytes. Herbicide recovery, peak resolution, and detector sensitivity were excellent without using column cleanup procedures.

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5.2 GHz 대역에서 동작하는 기억 기능 특성을 갖는 궤환 회로를 이용한 변환 이득 저잡음 증폭기 설계 (Design of Variable Gain Low Noise Amplifier with Memory Effects Feedback for 5.2 GHz Band)

  • 이원태;정지채
    • 한국전자파학회논문지
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    • 제21권1호
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    • pp.53-60
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    • 2010
  • 본 논문에서는 5.2 GHz에서 입력 신호의 크기에 따라 효율적으로 동작하는 저잡음 증폭기를 0.18 um CMOS 공정을 이용하여 설계하였다. 제안된 회로는 궤환 회로와 2단 저잡음 증폭기로 구성되어 있으며, 궤환 회로의 경우 7개의 함수 블록으로 구성되어 있다. 본 논문에서는 변화되는 신호 전압을 감지하는 것과 이전 상태를 기억하는 저장 회로에 초점을 두어 불필요한 전력 소비를 제거하였다. 기억 기능 특성을 갖는 궤환 회로의 출력값을 이용하여 통제되는 저잡음 증폭기는 11.39 dB에서 22.74 dB까지 변하며, 최고 이득 모드일 때 잡음 지수가 최적화 되도록 설계되었다. 변환 저잡음 증폭기는 1.8 V의 공급 전압에 대해서 5.68~6.75 mW를 소비한다.

벤지딘 및 벤지딘계 염료(Direct Black 38)의 요중 대사물질에 관한 연구 (A study on the urinary metabolites of benzidine and benzidine based dye(Direct Black 38))

  • 노재훈;원종욱;김치년;김현수;전미령
    • 한국산업보건학회지
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    • 제6권1호
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    • pp.156-164
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    • 1996
  • Benzidine is recognized as a urinary bladder carcinogen in humans. The use of benzidine in industries was prohibited because of its carcinogenecity, but, production and usage of benzidine-based dye was still permitted in most countries. This study was performed to compare the excretory patterns of urinary metabolites between benzidine-based dye(Direct Black 38) and benzidine in rats Benzidine-based dye was administered orally at the doses of 0.3, 0.5, 0.7 mmol/kg and benzidine was administered orally at the doses of 0.2, 0.4, 0.6 mmol/kg into Sprague-Dawley rats. To analyze benzidine and its metabolites, the high performance liquid chromatography with an electric chemical and ultraviolet detector were used. N-acetylbenzidine, N,N'-diacetylbenzidine and 4-aminobiphenyl were identified in the urine of the rats receiving dye and benzidine. The excreted amount of the urinary benzidine from dye was almost 1/10 of that from benzidine. Excretion rates of metabolites were more prolonged in the dye receiving group than those of the benzidine group. Peak concentration time of urinary N,N'-diacetylbenzidine was more prolonged than other metabolites in both groups. The excreted amount of N-acetylbenzidine was more than the others in both group. These results suggested that N-acetylbenzidine may be an useful Biological exposure index for benzidine-based dye.

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Solid Phase Microextraction을 이용한 계피의 향기성분 분석 (Analysis of Aroma Compounds of Cinnamon by Solid Phase Microextraction)

  • 이창국;이재곤;장희진;곽재진
    • 한국식품영양학회지
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    • 제16권4호
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    • pp.372-378
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    • 2003
  • SDE 및 SPME를 이용하여 계피로부터 추출한 휘발성 향기성분을 GC/MSD 분석한 결과 terpenes 20종, alcohol 3종, carbonyl 5종, esters 2종으로 총 30개의 휘발성 성분을 확인하였다. 이들 중 trans-cinnamaldehyde (86.4%), cis-cinnamaldehyde(0.9%), hydrocinnamaldehyde (0.1%) 등의 carbonyl 화합물이 peak area% 기준으로 약 88.2%로 계피 중 대부분을 차지하는 것으로 나타났다. 또한 식물체의 향기성분 분석에 많이 이용되는 SPME fiber 4종류를 비교 분석한 결과 terpen류 화합물들은 PDMS fiber에서 추출효율이 가장 좋았으며, cinnamyl alcohol과 같은 다소 극성인 화합물의 경우 DVB/CAR/PDMS fiber와 PA fiber에서 추출 효율이 가장 좋은 것으로 나타났다. SPME법에서 최적 조건을 설정하기 위해 추출온도와 추출시간을 달리하면서 비교 분석한 결과 copaene, murolene, cadinene, cis-cinnamaldehyde 등의 area% 값은 온도와 시간이 커질수록 증가한 반면에 trans-cinnamaldehyde의 area% 값은 감소하였다.

공기중 6가 크롬 측정 방법 비교 -검출한계, 정확도 및 정밀도- (Comparison of Sampling and Analytical Methods for Determining Airborne Hexavalent Chromium -Limit of Detection, Accuracy and Precision of Analytical Procedures)

  • 신용철;이병규;이지태
    • 한국대기환경학회지
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    • 제18권1호
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    • pp.39-49
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    • 2002
  • In this study, limits of detection (LOD), accuracy and precision of four sampling/ analytical methods were evaluated and compared for the determination of airborne hexavalent chromium, Cr (VI). The methods include : (1) a combination of the National Institute for Occupational Safety and Health (NIOSH) Method 7600/U. S. Environmental Protection Agency (EPA) Method 218.6 (NIOSH/EPA Method) proposed by Shin and Paik, 2) two impinger methods using 2% NaOH/3% Na$_2$CO$_3$. (3) same as (2) but with 0.02 N NaHCO$_3$absorbing solution, and (4) the Occupational Safety and Health (OSHA) Method ID-215. An ion chromatograph/visible absorbance detector was used for the analysis of Cr (VI) in sample solution. Limit of detection (LOD) , analytical accuracy, and precision were also tested using Cr (VI) spike samples. Recoveries (as index of accuracy) and coefficient of variation (CV) (as a index of precision) were determined. Two-way ANOVA and Turkey's test were performed to test the significance in differences among recoveries and CVs of the methods. In all the methods, the peaks of Cr (VI) were separated sharply on chromatograms and exhibited a strong linearity with Cr (VI) concentrations in solution. The correlation coefficients of calibration curves typically ranged from 0.9997 to 0.9999, and the analytical LODs from 0.025 to 0.1$\mu\textrm{g}$/sample. All the method had good sensitivities and linearities between Cr (VI) levels and peak areas. The accuracies (% mean recoveries) of the methods ranged from 80.1 to 104.2%, while the precisions (pooled coefficient of variation) ranged from 3.16 to 4.43%. The impinger methods showed higher recoveries ( > 95%) than those of the PVC filter methods (the OSHA Method and the NIOSH/EPA Method). It was assumed that Cr (VI) on PVC filter was exposed to air and reduced to trivalent chromium, Cr (III), whereas it was stabilized in alkali solution contained in impinger. Thus, a special treatment of Cr (VI) samples collected on PVC filters may be required.

HPLC 분석법을 이용한 이중탕(理中湯) 제제의 품질평가 (Quality Assessment of Ijung-tang Preparations Using a HPLC Analysis)

  • 하우람;박진형;윤동인;이장천;김정훈
    • 대한본초학회지
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    • 제31권3호
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    • pp.29-35
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    • 2016
  • Objectives : Ijung-tang (IJT) is a traditional herbal formula and has been used to treat digestive diseases such as abdominal pain, vomiting, and diarrhea. IJT consists of four herbal medicines, Ginseng radix, Atractylodis rhizoma alba, Zingiberis rhizoma, and Glycyrrhizae radix et rhizoma, containing various bioactive compounds. Quality assesment of IJT preparations was performed by analytical method for determining marker compounds.Methods : Determination of seven marker compounds in IJT preparations was quantitatively conducted by high-performance liquid chromatography equipped with a diode-array detector. The marker compounds were separated on a reversed-phase C18 column and the analytical method was successfully validated. Chemometric analysis was performed to compare IJT water extracts and commercial IJT granules.Results : Limit of detection and limit of quantification values were in the ranges of 0.093-2.649 μg/mL and 0.283-8.027 μg/mL, respectively. Precisions were 0.30-3.87% within a day and 0.23-2.35% over three consecutive days. Recoveries of the marker compounds ranged from 87.35-107.05%, with relative standard deviation (RSD) values < 6.15%. Repeatabilities were < 1.20% and < 1.71% of RSD value for retention time and absolute peak area, respectively. The results from quantitative analysis showed that the quantities of seven marker compounds of IJT samples varied, as were found in principal component analysis and hierarchical clustering analysis.Conclusions : The analytical method developed in the present study was precise and reliable to simultaneously determine marker compounds of IJT. Therefore, it can be used for the quality assessment of IJT preparations.

율무 지질의 Triglyceride 조성에 관한 연구 (Studies on the Triglyceride Composition of Job's Tears)

  • 이희자;조광연;배정설;장순욱
    • 한국식품조리과학회지
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    • 제6권4호통권13호
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    • pp.27-32
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    • 1990
  • Triglyceride는 구성지방산의 종류에 따라 분자종이 다양하게 존재하여 식품의 가공, 저장중에 있어서 유지의 물성변화 및 산화특성을 효과적으로 규명하기 위해서는 구성 triglyceride 분자종의 상세한 해석이 요구된다고 하겠다. 율무 지질의 triglyceride를 reverse phase HPLC UV detector 210nm에서 분석한 결과 6개의 peak로 분획되었다. 각 획분을 GC로 acycl 탄소수별로 분획하고, 다시 DEGS column을 이용하여 fatty acid 조성을 분석하였다. 이 세가지 결과로부터 triglyceride 조성을 산정한 결과 11개의 TG 조성을 추산하였으며, 그 중 주요 triglyceride로는 C18 : 1 C18 : 2 C18 : 2(OLL)이 38.2%, C16 : 0 C18 : 2 C18 : 3(PLLn)이 15.7%, C18 : 1 C18 : 1 C18 : 2(OOL)이 12.6%였다. 한편 capillary GC와 GC-MS로 같은 시료를 분석하여 분자종을 확인하는 작업을 계속하고 있으며 위의 결과와 비교하여 다음에 보고하고자 한다.

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9-Anthracenylmethyl 1-Piperazinecarboxylate(PAC)을 이용한 공기중 총이소시아네이트 분석방법 개발:제1부 반응조건 및 안전성 (Development of a New Method for Total Isocyanate Determination Using the Reagent 9-Anthracenylmethyl 1-Piperazinecarboxylate(PAC):Part 1 - The reaction condition and stability)

  • 노영만
    • 한국산업보건학회지
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    • 제9권2호
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    • pp.167-176
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    • 1999
  • A new analytical procedure for the measurement of monomeric isocyanates and total isocyanate group in workplaces has been investigated. The method described herd involves derivatization of the isocyanate sample upon collection with the reagent 9-anthracenylmethyl 1-piperazinecarboxylate (PAC). Laboratory investigations have demonstrated that excess PAC reagent can be satisfactorily removed from PAC-derivatized monomeric isocyanates-a requirement for the success f the analytical procedure. After removal of excess PAC reagent, the PAC derivatives of butyl isocyanate, phenyl isocyanate, HDI, MDI, and TDI were reacted with sodium thiomethoxide to convert them all to 9-anthracenylmethyl methyl sulfide (AMMS). Total isocyanate group was determined by HPLC analysis and quantification of the single AMMS peak. This circumvents many of the disadvantages associated with current HPLC methods. There were no longer problems associated with quantifying late-eluting peaks and analysis times were very short. A single detector was used for quantification because a standard of the analyte existed and the retention time could be determined. Because all species were converted to a single analyte, the problem of variability of response factors among different species was averted. Finally, there were no complex chromatograms to interpret. Monomers of other individual species were measured by analysis of the sample before the individual species were converted to AMMS. The favorable performance of PAC warrants its further study as a reagent for the determination of total isocyanate group in air.

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방아(Agastache rugosa O. Kuntze)의 향기성분 (Volatile Flavor Components of Bangah (Agastache rugosa O. Kuntze) Herb)

  • 안빈;양차범
    • 한국식품과학회지
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    • 제23권5호
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    • pp.582-586
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    • 1991
  • 방아의 휘발성 향기성분을 수증기 증류장치로 추출한 후 GC 및 GC/MS에 의하여 비교 분석하였다. 확인된 성분을 기능기 별로 보면 hydrocarbon류 14종, aldehyde류 6종, ketone류 5종, alcohol류 3종, phenol류 5종, ester류 2종, 기타 1종으로 총 36종의 향기성분이 확인 되었다. 이중에서 estragole이 90% 이상으로 가장 많이 함유되었고 그밖에 limonene($0.7{\sim}4.7%$), caryophyllene($0.9{\sim}1.1%$), eugenol($1.4{\sim}1.9%$), anethol($0.2{\sim}0.3%$)등이 주요성분이었다. 그러고 이들 향기성분의 종류 및 함량을 채취시기 별로 보면 어린잎보다 성숙된 잎에서 높게 나타났고, 부위별로는 꽃대에서 가장 높았고 잎, 줄기의 순으로 남아졌다.

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인공 항문계를 이용한 대두박 isoflavones의 생체 이용성 평가

  • 김경진;지규만
    • 한국가금학회:학술대회논문집
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    • 한국가금학회 2000년도 제17차 정기총회 및 학술발표
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    • pp.91-93
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    • 2000
  • Soybean meal(SMB) has not only been an important source of protein, but also a major source of isolfavones(IF) for poultry diet. Since the IF is one of effective phytoestrogens, evaluation of bioavailability of the phytochemicals for poultry and development of an animal model for assessment of the availability should be essential for its practical application. Present study was to develop bird model for assessing their bioavailability. No reports for such measurments with poultry could have every been found. Eight, 6-wk-old, layer-type, male birds were divided into two groups of four birds; normal (N) and colostomized(COL). Each bird was tube-fed a SMB sample at a level of 1% body weight. Samples from blood, urine and feces(COL birds) or urine+feces (N) were collected at 0, 2, 8, 15, 24 and 48 hours after the feeding. Plasma and urine samples were treated with -glucuronidase and fecal samples with 4N HCl for measurement of genistein(GE) and daidzein (DA) with HPLC set with an electrochemical detector. Maximum peaks of plasma IF appeared at 2 h after the meal for both birds groups. However the IF peak for N group was GE, while that for COL group was DA. Plasma DA levels for COL birds were always higher than those of GE, which was in opposite trend for N birds. This trend observed in the N birds is in accordance with those reported in rats fed SBM. In conclusion the results seem to suggest that colostomy as an attempt to separate urine from feces in birds affected the IF metabolism in the intestine and may not be a proper bird model to measure the IF bioavailability.

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