• 제목/요약/키워드: solid-phase extraction (SPE)

검색결과 200건 처리시간 0.028초

Part-Per-Trillion level determination of Alkylphenols, Chlorophenols and Bisphenol A using GC/MS-SIM in Tap Water

  • Kim, Hyub
    • 한국환경독성학회:학술대회논문집
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    • 한국환경독성학회 2003년도 추계국제학술대회
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    • pp.149-149
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    • 2003
  • A new technique is proposed for the determination of alkylphenols, chlorophenols and bisphenol A in tap water. The sample preparation consists of a solid phase extraction (SPE) of alkylphenols, chlorophenols and bisphenol A from a water sample with XAD-4 and subsequent conversion to isobutyloxycarbonyl (isoBOC) derivatives or tert.-butyldimethylsilyl (TBDMS) derivatives for sensitive analysis with the GC/MS-SIM mode. The recoveries were 86.6∼105.2 % (isoBOC derivatization) and 97.6∼484.5 % (TBDMS derivatization), respectively. The limit of quantitation of alkylphenols, chlorophenols and bisphenol A for SIM were 0.001∼0.050 $\mu\textrm{g}$/l (isoBOC derivatization) and 0.003∼0.050 $\mu\textrm{g}$/l (TBDMS derivatization). The SIM responses were linear with the correlation coefficient varying 0.9755∼0.9981 (isoBOC derivatization), and 0.9908∼0.9996 (TBDMS derivatization). The derivative methods and their application to tap water samples will be disscussed.

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Selective Concentration and Determination of Phenol and Chlorophenols by Solid Phase Extraction

  • Jung, Min-Woo;Lee, Dai Woon;Paeng, Ki-Jung
    • 분석과학
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    • 제8권4호
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    • pp.535-538
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    • 1995
  • This study employs the variety of mixtures of XAD resin and active carbons as concentration base for solid phase extraction (SPE) which has been widely used to preconcentrate and purify phenol and chlorophenols in determination of environmental water samples. In this study, we employed variety of mixtures of copolymer based XAD-4 resin with active carbons. This cartridges shows advantages of both materials, such as better affinity to phenol by active carbon and better mechanical stabilities from XAD resin. The better enrichment factor, pretreatment time, recoveries and limit of detection (LOD) were achieved by the attempts to pack precolumns with both meterials for preconcentration.

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Determination of Histamine in a Pharmaceutical Preparation after Clean-Up by Solid- Phase Extraction

  • Kim, Chang-Soo;Kim, Naml-Lee;Jeong, Min-Gyo;Hong, Seung-Hwa;Moon, Dong-Cheul
    • 대한약학회:학술대회논문집
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    • 대한약학회 2002년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2
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    • pp.397.1-397.1
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    • 2002
  • A human immune globulin preparation (histobulin\ulcorner) are made to bind a small amount of histamine (0.15 $\mu$g) to the protein (12 mg) to increase the resistance of histamine susceptibility in the treatment of allergic diseases. Strict control of histamine content of the drug are required since intake of histamine might result in hypo- or hypertension. headache. or anaphylactic shock syndromes. HPLC analytical method with pre-column fluorescent derivatizalion after clean-up by solid-phase extraction (SPE) was developed. (omitted)

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Characterization of Natural Organic Matter in Spring Water

  • Yoo, Hee-Jin;Choi, Yoon-Ji;Cho, Kun
    • Mass Spectrometry Letters
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    • 제11권4호
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    • pp.90-94
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    • 2020
  • Interest in aspects of industrialization relating to human health has increased. Accordingly, the use of labels such as 'natural foods' and 'organic ingredients' has become more widespread, and greater emphasis is being placed on improving quality of life. Water is an essential element for human life, and water quality has a significant impact on human health. However, technology that can precisely determine the substances present in water is still lacking. This study was conducted to establish a complete mass spectrometry process, from pretreatment to analysis, to measure and characterize natural organic matter (NOM) in Korean spring water samples. Salts and other matrices were removed from the samples using solid-phase extraction (SPE) with two different columns (PPL and C18). After establishing an accurate analysis method, the experimental results were evaluated based on Van Krevelen diagrams and analysis of molar O/C and H/C ratios. The method for characterizing NOM introduced herein should facilitate evaluation of water quality.

종이재 중의 Pentachlorophenol 정량 분석 (Quantitative Analysis of Pentachlorophenol in Paper Products)

  • 한애란;박지혜;최형기;홍성엽;한혜철;조병묵;오정수
    • 공업화학
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    • 제16권3호
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    • pp.323-327
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    • 2005
  • Pentachlorophenol (PCP)은 독성이 강한 발암성 물질로 미국환경청(Environmental Protection Agency, USA)이 정한 대표적인 환경호르몬이다. 본 연구에서는 종이 중에 함유된 극미량의 PCP 측정을 목적으로 하였다. 종이의 전처리는 고상추출법(SPE)을 이용하였고 분석을 위해 PCP를 유도체화시켜 gas chromatography/mass spectroscopy-selected ion monitoring (GC/MS-SIM)으로 분석하였다. GC/MS-SIM의 분석 결과 실릴화 PCP의 분석감도가 증가되었다. 본 실험에서는 실험군으로 사무용지와 벽지를 사용하였다.

Method development and initial results of testing for perfluorooctane sulfonate (PFOS) and perfluorooctanoic acid (PFOA) in waterproof sunscreens

  • Keawmanee, Sasipin;Boontanon, Suwanna Kitpati;Boontanon, Narin
    • Environmental Engineering Research
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    • 제20권2호
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    • pp.127-132
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    • 2015
  • Perfluorooctane sulfonate (PFOS) and Perfluorooctanoic acid (PFOA) are persistent environmental pollutants, extremely stable, and possibly adversely affect human health. They are widely used in many industries and consumer goods, including sunscreen products. These substances are stable chemicals made of long carbon chains, having both lipid- and water-repellent qualities. The research objectives are (1) to find the most effective method for the preparation of semi-liquid samples by comparing solid phase extraction (SPE) and centrifugation after Pressurized liquid extraction (PLE), and (2) to determine the contamination levels of PFOS and PFOA in waterproof sunscreen samples. All sunscreen samples were analyzed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Sunscreen samples were purchased from domestic and international brands sold in Thailand. Special chemical properties were considered for the selection of samples, e.g., those found in waterproof, sweat resistant, water resistant, and non-stick products. Considering the factors of physical properties, e.g., operation time, chemical consumption, and recovery percentage for selecting methods to develop, the centrifugation method using 2 mL of extracted sample with the conditions of 12,000 rpm and $5^{\circ}C$ for 1 hour after PLE was chosen. The highest concentrations of PFOS and PFOA were detected at 0.0671 ng/g and 21.0644 ng/g, respectively. Even though present concentrations are found at ng/g levels, the daily use of sunscreen products is normally several grams. Therefore, a risk assessment of PFOS and PFOA contamination in sunscreen products is an important concern, and more attention needs to be paid to the long-term effects on human health.

인삼의 진세노사이드 분석을 위한 추출 및 전처리법 (Extraction and Preprocessing Methods for Ginsenosides Analysis of Panax ginseng C.A. Mayer)

  • 김금숙;현동윤;김영옥;이성우;김영창;이승은;손영득;이민정;박충범;박호기;차선우;송경식
    • 한국약용작물학회지
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    • 제16권6호
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    • pp.446-454
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    • 2008
  • An advanced extraction method by ultrasonic extraction with applied solid phase extraction (SPE) has been developed for the determination of simultaneous eight major ginsenosides, namely ginsenosides Rg1, Re, Rf, Rb1, Rg2, Rc, Rb2, and Rd in the root of Panax ginseng. Four extraction methods including n-BuOH reflux extraction (Method A), 70% EtOH reflux extraction (Method B), 50% MeOH reflux extraction with SPE (Method C), and 50% MeOH ultrasonication with SPE clean-up process (Method D) were investigated for the determination of eight major ginsenosides. Total contents of ginsenosides were highest by extraction of Method C as $2.408{\pm}0.011%$. However, Method D was evaluated as relatively simpler and more efficient method due to short extraction time, small solvent consumption and less expensive, compared to conservative reflux method. Ginsenosides were also satisfactorily separated with good resolution and the accuracy range was between 1.05 and 4.06% as relative standard deviation (RSD) by Method D. SPE condition and HPLC condition were further optimized for determination of eight major ginsenosides by the ultrasonic extraction method. Conclusively, ultrasonic extraction of 2 g sample of ginseng using ultrasonic bath and 1 loading for SPE was evaluated as proper condition for extraction of ginseng.

고체상 추출과 친화 크로마토 그라피-유도결합 플라즈마 질량분석법을 이용한 한국인 혈청에서의 셀레노 단백질 정량 (Quantification of seleno proteins in Korean blood serum using solid phase extraction and affinity chromatography-inductively coupled plasma/mass spectrometry)

  • 안지윤;권효식;박용남
    • 분석과학
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    • 제27권2호
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    • pp.92-99
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    • 2014
  • 본 연구에서는 음이온 고체상 추출법 (AE SPE; anion exchange solid phase extraction)을 사용하여 간섭요인을 제거한 후, 친화 크로마토그래피 AF HPLC; affinity high performance liquid chromatography)와 유도결합 플라스마 질량분석법 (ICP/MS; inductively coupled plasma/mass spectrometry)을 사용하여 한국인의 혈청에서의 셀레노 단백질을 분리하고 정량하였다. 먼저 동위원소 희석법으로 셀레늄 총량을 분석한 결과, 건강한 한국 사람의 혈청내 평균농도는 $94.3{\pm}2.3ngg^{-1}$ 이었다. AE SPE와 AF 컬럼을 online으로 연결하여 셀레노단백질인 glutathione peroxidase (GPx), selenoprotein P (SelP), selenoalbumin (SeAlb)을 분리하고, 후 컬럼 동위원소 희석법 (PC ID; post column isotope dilution)으로 정량하였다. 혈청 인증표준물인 BCR-637을 분석한 결과 전체 셀레노 단백질의 합은 $85.4{\pm}3.4ngg^{-1}$으로 문헌값인 $81{\pm}7ngg^{-1}$과 일치하는 결과를 얻을 수 있었다. 20 명의 건강한 한국인의 혈청에서 얻은 셀레노 단백질 GPx, SelP 및 SeAlb 의 농도는 각각 $12.1{\pm}1.4ngg^{-1}$, $57.2{\pm}2.0ngg^{-1}$, 그리고 $20.0{\pm}1.9ngg^{-1}$ 이었으며 이들의 합인 $89.3ngg^{-1}$은 셀레늄의 총량값인 $94.3ngg^{-1}$과 거의 같은 값으로 혈청에서의 셀레늄은 주로 셀레노 단백질로 구성되어 있음을 알았다. 이 중 GPx의 농도는 간섭을 제거하기 전인 $25.0ngg^{-1}$에 비해 50% 이상 크게 감소하였는데 이로서 간섭은 주로 GPx에 포함되어 있음을 확인할 수 있었다. AE SPE는 간섭요인인 Cl과 Br을 제거 하는데 매우 효과적임을 보여주었다.

HPLC를 이용한 석유제품 중의 식별제 Unimark 1494DB 분석 (Determination of Unimark 1494DB in Petroleum using HPLC)

  • 임영관;김동길;임의순;신성철
    • Korean Chemical Engineering Research
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    • 제47권5호
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    • pp.593-598
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    • 2009
  • 정상경유에 등유 및 부생연료유를 인위적으로 혼합한 후, SPE 전처리 과정과 HPLC 분석을 통해 석유제품 내에 함유되어 있는 식별제의 정성 정량분석방법에 관해 연구하였다. SPE 전처리 과정에서 시료주입 후 15분에 분취된 시료에서 가장 높은 농도의 식별제가 분석되었다. 경유제품에 1 mg/L의 식별제를 혼입시킨 후, 전처리를 거쳐 HPLC로 분석한 결과 9.8분의 머무름시간에서 $1626.92mV{\cdot}sec$ 의 감도로 식별제가 분석되었으며, 또한 기존의 UV-Spectroscopy법으로 분석이 힘들었던 산성조건의 석유제품에서 식별제 분석이 가능하였다.

불산 중 극미량 음이온 분석을 위한 고상 추출법 및 이온크로마토그래프를 이용한 동시분석법 확립 (Optimization of solid phase extraction and simultaneous determination of trace anions in concentrated hydrofluoric acid by ion chromatography)

  • 윤석환;조동호;김현지;신호상
    • 분석과학
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    • 제29권5호
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    • pp.219-224
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    • 2016
  • A sensitive method to detect trace anions in hydrofluoric acid (HF) by solid-phase extraction (SPE) clean-up and ion chromatography (IC) was described. Fluoride in HF solution was eliminated with solid-phase extraction, and residual fluoride, acetate, chloride, bromide, nitrate, phosphate and sulfate were consecutively separated with IC. The SPE parameters (selection of adsorbent, sample volume and pH, elution solvent and its volume) were optimized and selected. The removal effect of fluoride in HF solution was the best on Oasis WAX column, and the optimum conditions (1.0 mL of 25 % HF solution and 50 mM ammonium acetate 5 mL as elution solvent) were established by the variation of parameters. Under the established condition, the method detection limits of chloride, bromide, nitrate, phosphate, and sulfate were 0.04~0.30 µg/L in 25 % HF solutions (w/w) and the relative standard deviation was less than 5 % at concentrations of 20.0 and 40.0 µg/L. The concentrations of anions in a 25 % HF had detectable levels of 4.2 to 47.5 µg/L. The method was sensitive, reproducible and simple enough to permit the reliable routine analysis of anions in HF solution used in the process of producing semiconductors.