• 제목/요약/키워드: Analytical determination

검색결과 1,490건 처리시간 0.026초

Simultaneous Determination of 4-Nitrotoluene and Benzophenone in Ground Water and Soil by Gas Chromatography-Mass Spectroscopy

  • Kwon, Oh-Seung;Kim, Eun-Young;Ryu, Jae-Chun
    • 분석과학
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    • 제16권1호
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    • pp.59-69
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    • 2003
  • Benzophenone (BZP) and 4-nitrotoluene (4-NT) listed as endocrine disrupting chemicals are suspected to contaminate ground water sites and soil. Analytical method for simultaneous determination of the two chemicals in soil and ground water was developed by gas chromatography-mass spectrometry. Water (100 ml) was extracted with hexane, and soil (10 g) was extracted with methanol and hexane. Recovery in water was >72% for BZP and 90-118% for 4-NT. Recovery for 4-NT and BZP in soil was 51-59% with coefficient variation of less than 19.5%. Calibration curves showed a good linearity with $r^2=0.997$. In water and soil collected at nation-wide sites, BZP was found at 5 sites among 43 water sites at the concentration of $14.87{\pm}3.83ng/100 ml$. No 4-NT was found. It is suggested that this method is appropriate to the simultaneous quantitation of 4-NT and BZP in ground water and soil samples.

중성자 방사화 분석법과 원자 분광법을 이용한 갯벌 시료 중 미량원소 분석법에 관한 연구 (Analysis of Trace Elements in Mud Flat with Neutron Activation Analysis (NAA) and Atomic Spectroscopy)

  • 남상호;김민재;정용삼;김선하
    • 분석과학
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    • 제15권6호
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    • pp.521-528
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    • 2002
  • 남해연안 갯벌 속에 있는 무기원소들의 정량을 위해 중성자 방사화 분석법과 ICP-AES를 적용하였다. 중성자 방사화 분석법과 ICP=AES에 의하여 얻어진 Al, Ca, Fe, Mg, K, Na의 분석결과들을 상호 비교하였다. 결과적으로 침전물 중의 미량 원소를 분석하는데 ICP-AES보다 중성자 방사화 분석법이 더 우수한 것으로 나타났다. 따라서 중성자 방사화 분석법은 갯벌과 같은 복잡한 모체를 갖는 환결시료들의 분석헤서 중요한 역할을 할 것이다.

Quantitative determination of 2'-Hydroxy-3',4'-methylenedioxy-3,4,5-trimethoxychalcone (HMTC) in rat plasma by HPLC-MS/MS and its application to a pharmacokinetic study

  • Jihyun Won;Juhyung Kang;Wonyoung Park;Jose C. J. M. D. S. Menezes;Marc Diederich;Eunyoung Kim;Wonku Kang
    • 분석과학
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    • 제36권1호
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    • pp.53-58
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    • 2023
  • 2'-Hydroxy-3',4'-methylenedioxy-3,4,5-trimethoxychalcone (HMTC) is a newly synthesized chalcone that affects proliferation, cytotoxic potential and apoptosis in human leukemia cells. However, no validated determination method has been described so far for HMTC in biological samples. Thus, we developed a liquid chromatographic method using a tandem mass spectrometry to determine HMTC in rat plasma. Liquid-liquid extraction with ethyl acetate was used for the clean-up procedure. The analyte was separated on a reversedphase column with mobile phase of distilled water and acetonitrile (2:8, v/v, including 0.1 % formic acid). The ion transition of the precursor to the product ion was principally deprotonated ions [M-H]- at m/z 356.8 → 327.2 for HMTC. This analytical method was successfully applied in pharmacokinetic study of HMTC after intravenous administration in rats.

2-Hydroxy-3-methoxy Benzaldehyde Thiosemicarbazone를 사용하여 마이크로 그램 코발트(II)의 직접 및 유도 분광광도법에 의한 정량 (Direct and Derivative Spectrophotometric Determination of Cobalt (II) in Microgram Quantities with 2-Hydroxy-3-methoxy Benzaldehyde Thiosemicarbazone)

  • Kumar, A.Praveen;Reddy, P.Raveendra;Reddy, V.Krishna
    • 대한화학회지
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    • 제51권4호
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    • pp.331-338
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    • 2007
  • 분석 시약으로 2-hydroxy-3-methoxy benzaldehyde thiosemicarbazone (HMBATSC)를 사용하여 코발트 (II) 정량을 위하여 빠르고 간단하고 민감한 분광광도법을 개발하였다. 액상에서 금속이온이 pH 6.0에서 HMBATSC와 갈색의 착물을 형성하였다. 이 착물은 375 nm와 390 nm에서 두 개의 최대 흡수 피크를 보였다. 375 nm에서 많은 흡 수를 보였고, 반면 390 nm에서는 분명한 흡수를 보이지 않았다. Beer's 법칙에서 Co(II)는 0.059-2.357 μg ml-1 범위를 보였다. 이 방법의 몰 흡수와 Sandall's 민감도는 각각 2.74×104 l mol-1 cm-1와 0.0024 μg cm-2 였다. 여러 가지 다른 이온들에 간섭에 대해서도 연구하였다. 화학양론적으로 착체는 1:2 [Co(II)- HMBATSC] 이 였다. 이차 유도 분광광도 법에 의한 Co(II)의 정량방법에 대해서도 제안하였다. 제안된 방법을 alloy steels, 비타민 B12와 생물학 시료에 있는 Co(II)의 정량에 적용하였다.

기체크로마토그래피/질량분석법을 이용한 생체시료 중 Polybrominated Biphenyls의 분석법 (Determination of Polybrominated Biphenyls in Biota Samples Using Gas Chromatography/Mass Spectrometry)

  • 홍종기;백인걸;김협;김도균;서정주;서종복;박현미;이강봉
    • 분석과학
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    • 제13권5호
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    • pp.666-674
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    • 2000
  • 본 연구는 기체크로마토그래피-질량분석법을 이용한 생물시료 중 polybrominated biphenyls(PBBs)의 분석법을 설명하였다. 생물 시료 중 PBB류는 40mL 아세톤과 80mL의 헥산 혼합용매에서 초음파추출기 20분간 교반하여 추출하였다. 추출액 중 존재하는 지질성분은 농축 황산용액으로 분해한 후 PBB류는 Florisil 컬럼으로 정제하였다. PBB류를 정량분석하기 위하여 정제액은 GC/MS-selected ion monitoring 방법에 의해 분석하였다. 본 실험 조건하에서 전반적인 PBB류의 추출율은 77-111%로 나타났다.

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Qualitative and quantitative determination of oleanolic acid in a scalp tonic products by HPLC using response surface methodology for extraction optimization

  • Cai, Lin Xi;Cho, Chong Woon;Zhao, Yan;Kang, Jong Seong;Kim, Kyung Tae;Jung, Sang-Hun
    • 분석과학
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    • 제32권2호
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    • pp.48-55
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    • 2019
  • The simple and effective analytical method for the quality control of a novel scalp tonic formulation has been developed and optimized in terms of HPLC conditions and sample preparation method, meanwhile, the optimization of preparation condition was using response surface methodology (RSM) based on central composite design (CCD). Oleanolic acid was selected as marker compound because of its bioactivities for alopecia therapy. The developed analytical method and extraction condition were successfully qualified. Coefficient of determination ($r^2$) for the calibration was 0.9997 with a line passing through the origin point in the range of 0.1-100 mg/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) were 17.5 ng/mL and 55.0 ng/mL, respectively. The intra-day and inter-day precision of the method were 0.5-1.4 % and 0.7-1.8 % in relative standard deviation, respectively, while those accuracy were 99.5-100.9 % and 100.0-102.2 %, respectively. The repeatability of oleanolic acid in samples ranged of 0.3-1.9 % based on peak area and 0.3-0.7 % for retention time. Recoveries from samples were 95.0-99.4 % with lower than 1.8 % in relative standard deviation. Overall, the developed analytical method will be used for quality control of this commercial scalp tonic products successfully.

The Significance of the Analytical Sciences In Environmental Assessment

  • Chung, Yong;Ahn, Hye-Won
    • 분석과학
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    • 제8권4호
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    • pp.1079-1087
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    • 1995
  • The quality of human life is directly related to the quality of the environment. To assess environmental quality we must first determine the MCLG(Maximum Contaminant Level Goal), MCL(Maximum Contaminant Level), environmental impact and so on. The MCLG is the concentration at which no known adverse health effects occur. The MCLG is determined by risk assessment identifying which process is hazardous assessing, dose-response, human exposure, and characteristics of risk. With consideration of analytical methods, treatment technology, cost and regulatory impact, the MCL is set as close to the MCLG as possible. In this way, determination of the concentration and national distribution of contaminants is important for assessment of environmental quality The analytical sciences pose potential problems in assessing environmental quality. Continuing improvement in the performance of analytical instruments and operating technique has been lowering the limits of detectability. Contaminant concentration below the detection limit has usually been reported as ND(Not-Detected) and this has often been misunderstood as equivalent to zero. Because of this, more the contaminant concentration in the past was below the detection limit, whereas contaminants can be quantified now even though the contaminant concentration might remain the same or may even have decreased. In addition, environmental sampling has various components due to heterogeneous matrices. These samples are used to overestimate the concentration of the contaminant due to large variability, resulting in excess readings for MCL. In this paper, the significance of the analytical sciences is emphasized in both a conceptual and a technical approach to environmental assessment.

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기체크로마토그래피/질량분석기에 의한 수질, 토양 및 저질 시료중의 benzophenone 분석법에 관한 연구 (Determination of benzophenone in water, soil and sediment by gas chromatography/mass spectrometry)

  • 전희경;최해연;류재천
    • 분석과학
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    • 제18권2호
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    • pp.147-153
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    • 2005
  • 본 연구는 GC/MS를 이용하여 수질, 토양 및 저질 시료 중의 benzophenone (BP)을 분석하는 방법을 확립하고자 하였다. BP는 수질 시료 (100 mL)에서 n-hexane으로 추출하였으며, 토양 및 저질 시료 (10 g)에서는 먼저 메탄올로 추출한 후 hexane으로 다시 추출하여 농축시켜 분석하였다. 수질 시료 중의 BP 회수율은 71.4% 이상이었으며 토양에서의 회수율은 86.5-94.7%를 보였고 재현성은 19.8% 이하였다. 검정곡선은 상관계수 ($r^2$) 값이 수질과 토양 모두에서 0.998이상의 좋은 직선성을 보여주었다. 수질 시료의 경우 43지역 중 3지역의 수질에서 30-200 ng/L 농도 범위로 BP가 검출되었으며 토양과 저질 시료에서는 모든 지역에서 검출되지 않았다. 이 분석방법은 환경 중에 미량으로 존재하는 BP의 분석과 모니터링에 유용하게 사용할 수 있는 적합한 방법이라 사료된다.

ESTIMATION OF SUGAR AND REDUCING SUGAR IN MOLASSES USING NEAR INFRARED REFLECTANCE SPECTROSCOPY

  • Mehrotra, Ranjana;Gupta, Alka;Tewari, Jagdish;Varma, S.P.
    • 한국근적외분광분석학회:학술대회논문집
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    • 한국근적외분광분석학회 2001년도 NIR-2001
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    • pp.1258-1258
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    • 2001
  • Estimation of sugar and reducing sugar content in molasses is very important task in sugar refineries. Conventional methods of determination of sugar content in molasses samples are highly time consuming and employ hazardous chemicals. Due to the physical properties of molasses, probability of error in conventional analytical techniques is high. These methods have proven to be inefficient for a process control in any sugar industry. Hence development of a rapid, inexpensive, physical and also accurate method for sugar determination in molasses will be highly useful. Near Infrared spectroscopy is being widely used worldwide as an analytical technique in food industry. The technique offers the advantage of being non-destructive and rapid. The present paper highlights the potential of near infrared reflectance spectroscopy as a rapid and automated analytical technique for determination of sugar and reducing sugar content in molasses. A number of molasses samples were collected during and after the sugar season from Havana Sugar Industry, Havana. The samples were chosen so as to obtain a wide range of concentration of sugar and reducing sugars. This was done in order to achieve a good calibration curve with widely spread data points. These samples were scanned in the region of 1100 - 2500 nm in diffuse reflectance mode. An indigenous ELICO NIR spectrophotometer, modified according to the requirements of sugar industry was used for this purpose. Each sample was also analyzed simultaneously by standard chemical methods. Chemical values were taken as reference for near infrared analysis. In order to obtain the most accurate calibration for the set of samples, various mathematical treatments were employed. Partial Least Square method was found to be most suitable for the analysis. A comparison is made between the actual values (chemical values) and the predicted values (NIR values). The actual values agree very well with the predicted values showing the accuracy of the technique. The validity of the technique is checked by predicting the concentration of sugar in unknown molasses samples using the calibration curve. The present investigation assesses the feasibility of the technique for on-line monitoring of sugars present in molasses in sugar industries.

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