• 제목/요약/키워드: gas chromatography-nitrogen phosphorus detector

검색결과 28건 처리시간 0.027초

Capillary Column Gas Chromatography/Nitrogen Phosphorus Detector를 이용한 흥분제 및 마약성 진통제의 동시분석에 관한 연구 (Simultaneous Analysis of Stimulants and Narcotic Analgesics by Capillary Column Gas Chromatography with Nitrogen Phosphorus Detector)

  • 노동석;신호상;강보경;백형기;김승기;이정애;김영림;박종세
    • 대한화학회지
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    • 제35권6호
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    • pp.659-666
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    • 1991
  • 질소를 함유한 흥분제와 마약성 진통제 18종류의 약물들을 gas chromatography-nitrogen phosphorus detector(GC-NPD)를 사용하여 human urine으로부터 동시에 신속하게 분석할 수 있는 최적조건을 찾기 위하여 pH 변화와 추출용매 변화에 따른 회수율을 조사하였다. pH 8.5에서 에테르를 추출용매로 사용하였을 때 가장 적은 방해영향과 가장 좋은 회수율을 나타냈다. NPD에 대한 각 약물들의 상대 감응인자를 구하였고, 이 상대감응인자는 약물이 가지고 있는 질소원자의 갯수가 증가할수록 작은 값을 나타냈다. 생체시료 중의 약물들을 신속하게 검정하기 위하여 내부표준물질인 diphenylamine에 대한 relative retention time(RRT)을 작성하였다. 상대머무름 시간은 0.1% 이하의 정밀도를 나타냈다.

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유기농약 분석을 위한 Multi-Pesticide Residue Method (Multi-Pesticide Residue Method for Organopesticide Analysis)

  • 김우성;이봉헌
    • 한국환경과학회지
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    • 제6권4호
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    • pp.385-389
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    • 1997
  • 농약 잔류물을 70% acetone으로 추출한 다음 dichloromethane 층으로 옮겨 추출물을 florisil과 alumina-N으로 충진시켜 column chromatography를 행하였다. 마지막 추출물을 electron-capture detector(GC/ECD)와 nitrogen-phosphorus detector(GC/NPD)를 가진 GC로 분석하였다. 분석 결과 17 가지의 유기염소계 농약과 15 가지의 유기인계 농약의 회수율이 각각 60.8 에서 84.9%와 70.5에서 100.0%의 범위이었으며(phosmet와 azlnphos-methyl은 제외) 본 분석 방법의 최소 검출 준위도 낮았다(0.021-0.058mg/kg).

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Quantitative Analysis of Tiropramide in Human Blood by Gas Chromatography with Nitrogen-Phosphorus Detector

  • Kwon, Oh-Seung;Park, Young-Jin;Ryu, Jae-Chun;Chung, Youn-Bok
    • Archives of Pharmacal Research
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    • 제26권5호
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    • pp.416-420
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    • 2003
  • The analytical method of antispasmodic agent tiropramide {$(\pm)\alpha$-(benzoylamino)-4-[2-(diethylamino)ethoxy]-N,N-dipropylbenzenepropanamide hydrochloride} was developed by gas chromatography/nitrogen-phosphorus detector (GC/NPD) in human plasma. Two kinds of tiropramide tablets were orally administered to volunteers by Latin square crossover design, and blood was withdrawn as designed schedule. The plasma of 1 mL was loaded on Sep-pak $C_{18}$ cartridge and eluted with methanol after washing with 30% methanol. The residue dissolved in 100 $\mu$L of methanol after evaporation was analyzed by GC/NPD. Precision (CV%) of intra-day was located within 2.6% and accuracy was less than 9.7%. Inter-day precision was below 8.7% and accuracy was relatively good as less than 14%. Plasma samples obtained from human volunteers were analyzed for the determination of tiropramide concentration by using this method. The method was sensitive, rapid and suitable enough to be applied for pharmacokinetic and bioequivalence studies of tiropramide in human volunteers.

유기인제 농약 분석 방법 (Multi-Pesticide Residue Method) 개발에 관한 연구 (Study on the Development of Analytical Method (Multi-Pesticide Residue Method) for Organophosphate Pesticides)

  • 이봉헌;김우성
    • 한국환경과학회지
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    • 제6권2호
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    • pp.183-187
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    • 1997
  • 유기인제 농약을 70% acetone으로 추출한 다음 dlchloromethane 층으로 옮겨 추출물을 florisil로 충진된 open-column에서 chromatography를 행하였다. 마지막 추출물을 nitrogen-phosphorus detector(GC/NPD)을 가진 GC로 분석하였다. Narrow-bore capillary GC(Ultra-2)에 대해 18 가지의 유기인제 농약의 회수율이 88.7%에서 100.0%에 달하였다. 본 분석 방법의 최소 검출 준위는 0.019 - 0.035 mg/kg 이었으며 sample throughput(추출, open-column chro-matography 및 GC 분석)도 상당히 개선되었다.(sample당 8시간)

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Multi-Pesticide Residue Method for Analysis of Organochlorine and Organophosphorus Pesticide

  • Bonghun Lee;Woo
    • 한국환경과학회:학술대회논문집
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    • 한국환경과학회 1997년도 가을 학술발표회 프로그램
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    • pp.37-39
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    • 1997
  • Pesticide residues were extracted with 70% acetone and transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil and alumina-N, The final extract was analyzed by gas chromatography with electron-capture detector(GC/ECD) and nitrogen-phosphorus detector(GC/NPD). Recoveries of the 17 organochlorine pesticides were ranged from 60.8 to 84.9% and those of 15 organophosphorus pesticides, from 70.5 to 100.0%(except phosmet and azinphos-methyl). The minimum detectable levels of this analytical method were low (0.021-0.058 mg/kg).

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Comparative Free and Acetylated Polyamine Profiles in the Urine of Normal Subjects and Various Cancer Patients

  • Suh, Ja Won;Lee, Seon Hwa;Park, Young Han;Chung, Bong Chul;Park, Jongsei
    • 분석과학
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    • 제8권4호
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    • pp.895-900
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    • 1995
  • Urinary free and acetylated polyamine profiles have been investigated for their potential usefulness as biochemical markers of cancer in a control of group comprised of healthy volunteers (32 cases) and patients with various types of cancers(48 cases). The nine (5 free and 4 acetylated) endogeneous polyamines were simultaneously determined by a sensitive capillary gas chromatography/nitrogen-phosphorus detector (GC/NPD). The newly modified (simple and convenient) method was developed and the compounds were isolated by adsorption onto silica gel and derivatized by heptafluorobutyric anhydride to enhance their specificity on gas chromatograms. The good quality-control data were obtained through the precision and accuracy test and the recovery range of them was 48.6 ~ 101.2 %. The Korean reference values of urinary polyamines were established and significant differences were found in cancer patients compared with normal subjects. Also, to eliminate subject variations, precursors to product concentration ratios were compared between cancer patients and control group. The ratios of both putrescine to spermidine and total (free plus acetylated) putrescine to total spermidine were significantly greater in cancer patients than in normal subjects.

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우리나라 하수 및 폐수 처리 슬러지의 유기인계 살충제의 함량 (Contemporary Organic Contamination Levels in Digested Sewage Sludge from Treatment Plants in Korea : (3) Organophosphorus Insecticides)

  • 홍기훈;이강영;정창수;이현경
    • 한국환경과학회지
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    • 제15권3호
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    • pp.229-236
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    • 2006
  • Organophosphorus pesticides (OPPs) contents in the sewage sludge derived from the residential and industrial areas were determined in order to characterize contemporary organic contamination levels as a part of the ongoing development of the environmentally sound sewage sludge management strategy in Korea. OPPs were extracted from freeze-dried sludges in a ultrasonic extractor. The extracts were cleaned-up by florisil column and subsequently fed into gas chromatograph/nitrogen phosphorus detector (GC/NPD) for determining OPP contents. Diazinon, dimethoate, disulfoton, EPN, malathion, methyl parathion, parathion, phorate and sulfotep were present in the appreciable amount in the domestic sewage sludges. The sum of the 9 OPPs in the sewage sludge varied from 534.8 to 15552.1 ${\mu}g/kg$, dry wt..

Determination of Formaldehyde in Cigarette Smoke and Inhibitory Effect of Plant Volatile Extracts on the Formation of Formaldehyde

  • Her, Jae-Young;Jang, Hae-Won;Lee, Kwang-Geun
    • Food Science and Biotechnology
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    • 제18권2호
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    • pp.471-474
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    • 2009
  • Formaldehyde (FA) is a carcinogenic compound present in cigarette smoke. In this study, the amount of formaldehyde was analyzed in 5 kinds of cigarettes and the inhibitory effect of plant volatile extracts on the formation of FA was investigated. After extraction of the cigarette sample, FA was converted into its thiazolidine derivatives by reaction with cysteamine, and then measured using a gas chromatography-nitrogen phosphorus detector (GC-NPD). The concentrations of FA in cigarette smoke were found between 138.24 and $217.82{\mu}mol/g$ cigarette smoke. Extracts isolated from Welsh onion (Allium cepa L.), garlic (Allium sativum L.), crown daisy (Chrylsanthemum coronarium L.), green pepper (Capsicum annuum L.), and sesame dropwort (Oenanthe javanica DC) were used for analyzing their inhibitory effects on the formation of FA. The inhibitory effects of extracts of Welsh onion, garlic, crown daisy, green pepper, and sesame dropwort on the formation of FA were 64, 47, 38, 47, and 19%, respectively.

Assay of Midazolam in Human Plasma by Gas-Liquid Chromatography with Nitrogen-Phosphorus Detection

  • 신호상;홍춘표;Yun-Suk Oh-Shin;강보경;이경옥;이규범
    • Bulletin of the Korean Chemical Society
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    • 제19권5호
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    • pp.524-526
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    • 1998
  • A sensitive and specific method is described for the determination of midazolam in human plasma. The drug was extracted from 1 mL of carbonate buffered plasma (pH 9.6) with 8 mL of diethyl ether. Famprofazone was used as internal standard. The organic phase was evaporated to dryness. The residue was dissolved in methanol for the direct analysis by gas chromatograph-nitrogen phosphorus detector system. In the concentration range of 1-5000 ng/mL, the calibration curve was linear. The coefficients of variation from the precision test were <6% at the range of the concentration of 0.10-2.00 μg/mL and the detection limit for midazolam in 1 mL of plasma was o.5 ng. This assay is more sensitive, selective, simple and rapid than earlier methods. Plasma midazolam concentrations were determined by this method after administration of midazolam.

기체 크로마토그래피/질소-선택적 검출을 이용한 소변 중 니코틴과 코티닌의 동시 분석 (Simultaneous Determination of Urinary Nicotine and Cotinine Using Gas Chromatography/Nitrogen-Selective Detection)

  • 김희갑;박미진
    • Environmental Analysis Health and Toxicology
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    • 제16권4호
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    • pp.181-188
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    • 2001
  • A gas chromatographic method was established for the simultaneous determination of urinary nicotine and cotinine. The analytes in basified urine containing a sufficient amount of Na$_2$S0$_4$were extracted into dichloromethane by vigorous shaking. Into the transferred organic phase was added a small amount of acidified methanol (0.5 N HCI in methanol), followed by concentrating the mixture to dryness using a mild stream of nitrogen gas. The concentrate was reconstituted with methanol and the final solution analyzed using the gas chromatograph equipped with the nitrogen-phosphorus detector. The reproducibility tests showed coefficients of variation less than 11% for both compounds. The percent recovery for both analytes ranged from 88 to 103%. The estimated method detection limits for nicotine and cotinine were 0.60 and 5.1 ng/mL, respectively. Extraction efficiencies for both nicotine and cotinine apparently declined without the addition of Na$_2$S0$_4$into the urine. Moreover, the absence of methanolic HCI in the extract resulted in almost complete evaporation of nicotine and partial loss of cotinine during the concentration process, indicating that the formation of nicotine-HCI and cotinine-HCI species is prerequisite to the suppression of the loss of both compounds.

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