• 제목/요약/키워드: SPE1

검색결과 343건 처리시간 0.032초

Application of Solid Phase Microextraction to the Analysis of Pesticides in Vegetables

  • Cho Tae-Hee;Kang Hee-Gon;Kim Tae-Rang;Chang Min-Su
    • 한국식품위생안전성학회:학술대회논문집
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    • 한국식품위생안전성학회 2001년도 The Asia-Pacific Conference on Reproductive Biology and Environmental Sciences
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    • pp.171-174
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    • 2001
  • Solid phase micro-extraction (SPME), a solvent-free, rapid and inexpensive method for the extraction of organic compounds from aqueous sample matrices, was evaluated for determination of the 120 pesticides in vegetables such as crown daisy, perilla leaf, leafy lettuce and to mato. The analysis conditions were chosen for the SPME method: 15 min of immersion of the PDMS fiber in 10 ml of the solution with stirring at 1,000 rpm. The recovery tests were carried out in triplicate. The range of recoveries was 0-142% for organochlorine pesticides and $4.9\sim200\%$ for organophosphorus pesticides. The recoveries were very low in the pesticide groups with low solubility in water. The recoveries became lower in proportion to the interference materials in vegetables. The recovery in tomato was relatively higher than that in perilla Ie af and crown daisy. The recovery values obtained by SPE and SPME were compared. In leaf y lettuce, recovery obtained by SPE method ranged from $58.1\%\;to\;136.1\%$ and recovery by SPME ranged from $9.6\%\;to\;176.3\%$ In organophosphorus pesticides. The recovery in SPME method was satisfactory with $136\%$ for ethoprophos, $119\%$ for methidathion and $113\%$ for diazinon. Meanwhile, recovery of EPN, phenthoate and 2,4-DDT revealed relatively low value of $38\%,\;41\%\;and\;3.4\%,$ respectively. However, most of pesticides applied to SPME method sho wed constant recovery and precision. From these results, it can be concluded that solid phase micro-extraction might be an appropriate method for the screening test of pesticides in vegetables.

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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.

GC/MS/MS를 이용한 105종의 잔류농약 분석에 관한 연구 (Determination of 105 pesticide residues by GC/MS/MS)

  • 김우성;도정아;이희정;이주영;양승주;이선희
    • 분석과학
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    • 제23권4호
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    • pp.395-404
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    • 2010
  • 레몬과 콩 그리고 채소류에서 105개의 잔류농약을 다종 다성분 분석법으로 GC/MS/MS 분석하였다. 각 시료로부터 acetonitrile로 1차 추출하고 NaCl 15 g을 첨가한 다음 액-액 분배하였으며, Florisil 고체상(SPE) Cartridge로 정제하여 분석하였다. 레몬과 콩에서의 105개 농약의 회수율은 azinphos-methyl, famoxadone, fenamidone, flufenoxuron, triadimefon을 제외한 모든 농약에서 우수한 것으로 나타났는데 레몬에서 71.1~126.0%, 콩에서는 72.5~124.5% 였다. 또한 레몬에서의 검출한계와 정량한계는 각각 0.001~150 ng/mL와 0.004~500 ng/mL으로 확인되었다.

Impact of Changes in Maternal Age and Parity Distribution on the Increasing Trends in the Low Birth Weight and Very Low Birth Weight Rates in South Korea, 2005-2015

  • Oh, Yujin;Bae, Jisuk
    • Journal of Preventive Medicine and Public Health
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    • 제52권2호
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    • pp.123-130
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    • 2019
  • Objectives: The aim of this study was to evaluate the impact of shifts in maternal age and parity on the increasing trends in the low birth weight (LBW) and very low birth weight (VLBW) rates from 2005 to 2015 in South Korea. Methods: Data from 4 993 041 live births registered with Statistics Korea during the period between 2005 and 2015 were analyzed. Applying a modified standardization method, we partitioned the total increment in the LBW and VLBW rates into (1) the increase in the LBW and VLBW rates due to changes in the maternal age and parity distribution (AP-dis) and (2) the increase due to changes in the age-specific and parity-specific rates (AP-spe) of LBW and VLBW for singleton and multiple births, respectively. Results: During the study period, the total increment in the LBW and VLBW rates was 1.43%p and 0.25%p, respectively. Among singleton births, changes in the AP-dis accounted for 79% (0.34%p) and 50% (0.06%p) of the total increment in the LBW and VLBW rates, respectively. Meanwhile, among multiple births, changes in the AP-dis did not contribute to the increase in the LBW and VLBW rates, with 100% of the increase in the LBW (1.00%p) and VLBW (0.13%p) rates being attributed to changes in the AP-spe. Conclusions: This study demonstrated that shifts in maternal age and parity were prominent contributors to the increase in the LBW and VLBW rates among singleton births between 2005 and 2015 in South Korea.

추출방법들에 의한 Malachite Green과 Leucomalachite Green 회수율 (Extraction Methods for Recovering Malachite Green and Leucomalachite Green)

  • 배진한;윤영수;윤성호;최광진;이정선;임치원;김연계;박희연
    • 한국수산과학회지
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    • 제41권1호
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    • pp.13-19
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    • 2008
  • Malachite green (MG), a triphenylmethane dye, is carcinogenic, mutagenic, teratogenic, a respiratory toxin, and causes chromosomal fractures. It is not permitted for use as an aquaculture veterinary drug in a number of countries. Sensitive extraction methods for MG and leucomalachite green (LMG), which have long residence times in fish tissues, were developed. For LMG, the average recovery of liquid extraction (LE) ranged from 41.71 (yellowtail) to 71.60% (snakehead); the recovery of liquid-liquid extraction (LLE) was between 67.68 (yellowtail) and 83.68% (snakehead); and the average recovery of solid-phase extraction (SPE) ranged from 84.16 (yellowtail) to 92.92% (shrimp). The recovery of MG was less than 30% with SPE. However, the dye is found primarily as the colorless reduced leuco form in fish tissues.

UV를 적용한 역삼투막의 실란-에폭시 표면 개질 및 특성 평가 (Characterization of Reverse Osmosis Membrane Surface Modified by Silane-epoxy Using UV)

  • 박희민;양원용;이용택
    • 멤브레인
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    • 제28권3호
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    • pp.169-179
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    • 2018
  • 본 연구는 역삼투막의 물리-화학적 표면 개질을 통하여 친수성 증가에 따른 내오염성 및 내염소성을 향상하고자 하였다. 자외선조사로 상용막 표면을 활성화한 후 실란 커플링제를 sol-gel법으로 개질하여 염소에 대한 민감도를 낮춰 폴리아마이드 활성층을 보호하여 내염소성을 향상시켰다. 또한, 에폭사이드의 개수가 다른 PGPE, SPE 두 종류의 에폭시로 코팅 후 에폭사이드의 개환반응으로 내오염성을 향상시켰으며, 표면 개질 조건은 접촉각과 FT-IR, XPS 분석을 통해 최적화하였다. 실란-에폭시 개질막의 오염성 평가 결과 투과도 감소율이 상용막보다 약 1.5배 감소하였고, 내염소성 평가 결과 $20,000ppm{\times}hr$에서도 염제거율이 90% 이상 유지되었다.

Comparison of Preparation Methods for the Quantification of Ginsenosides in Raw Korean Ginseng

  • Hong, Hee-Do;Sim, Eun-Mi;Kim, Kyung-Tack;Rho, Jeong-Hae;Rhee, Young-Kyung;Cho, Chang-Won
    • Food Science and Biotechnology
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    • 제18권2호
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    • pp.565-569
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    • 2009
  • This study was conducted to evaluate the effects of different preparation methods on the recovery and quantification of ginsenosides in raw Korean ginseng (Panax ginseng C.A. Meyer). Eight major ginsenosides ($Rb_1$, $Rb_2$, $Rb_3$, Rc, Rd, Re, Rf, and $Rg_1$) were analyzed by high performance liquid chromatography (HPLC), after which the recovery and repeatability of the extraction of those ginsenosides using 3 different preparation methods were compared [A. direct extraction (DE) method, hot MeOH extraction/evaporation/direct dissolution; B. solid phase extraction (SPE) method, hot MeOH extraction/evaporation/dissolution/$C_{18}$ cartridge adsorption/MeOH elution; C. liquid-liquid extraction (LLE) method, hot MeOH extraction/evaporation/dissolution/n-BuOH fractionation]. Use of the DE method resulted in a significantly higher recovery of total ginsenosides than other methods and a relatively clear peak resolution. Use of the SPE and LLE methods resulted in clearer peak resolution, but lower ginsenoside recovery than the DE method. The LLE method showed the lowest ginsenoside recovery and repeatability among the 3 methods. Given that the DE method employed only extraction, evaporation, and a dissolution step (avoiding complicate and time consuming purification), this technique may be an effective method for the preparation and quantification of ginsenosides from raw Korean ginseng.

수치에 의한 황금의 성분변화 (Change of Flavonoid Composition in Scutellaria baicalensis by Processing)

  • 김장희;양기숙;김태희
    • 약학회지
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    • 제43권1호
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    • pp.16-22
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    • 1999
  • Scutellaria baicalensis Georgi (Labiatae) has been extensively used in treatment of diarrhea, conjunctivitis, gastritis, enteritis and skin disease. As instructed in old description, the Scutellariae Radix should sometimes be processed before use. To 노디 light on the changes of chemical compositions by processing as well as processing method-activity relationships, Scutellariae Radix was heated at 16$0^{\circ}C$-20$0^{\circ}C$ for 30 min. in furnace or soaked with 20% EtOH (SPE) and boy's urine(SPU), respectively, which are one of processing methods and then heated at 17$0^{\circ}C$ for 30 min. To isolate the chemical components, Scutellariae Radix with/without processing were extracted with EtOH and EtOH extract was fractionated with ether, ethyl acetate and butanol to give respective fractions. Ether and EtOAc fractions obtained from the processed drug with urine (SPU) were subjected to chromatography to obtainsix components, oroxylin A, Wogonin, chrysin, baicalein, baicalein 7-O-$\beta$-D-glucopyranoside and $\beta$-sitosterol 3-O-$\beta$-D-glucopyranoside. All the isolated compounds were identified by means of physicochemical and spectroscopic methods (IR, $^1H-NMR,{\;}^13C-NMR$, Mass). By HPLC determination, the changes of the contents for each isolated components from SPE and SPU samples were observed. It was found that the content of nonglycosidic flavones such as oroxylin A, wogonin, chrysin and baicalein was increased markedly, whereas the content of baicalin and baicalein 7-O-$\beta$-D-glucopyranoside was significantly decreased in both samples as compared with those of Scutellariae Radix. When the sample was soaked with boy's urine, the total amount of nonglycosidic flavones was higher than that of processing with 20% EtOH.

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UPLC를 활용한 데리스 추출물 함유 유기농자재 중 Rotenone과 Deguelin 정량분석 (Quantitative Analysis of Rotenone and Deguelin in Biopesticides Containing Derris Extract by Ultra performance Liquid Chromatography)

  • 임성진;김진효;최근형;박병준
    • 한국환경농학회지
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    • 제34권1호
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    • pp.52-56
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    • 2015
  • BACKGROUND: Three commercial biopesticides containing derris extract, which is permitted as a commercial biopesticide substances by the Environmentally-friendly Agriculture Promotion Act, have been marketed in Korea. But, the quantitative analytical method of active substances for crop protection in biopesticides containing derris extract has not known. METHODS AND RESULTS: Solid phase extraction (SPE) cartridge clean-up method for the quantitative analysis of rotenone and deguelin in biopesticides containing derris extract was developed and validated by ultra-performance liquid chromatography (UPLC). The clean-up method was established using hydrophilic lipophilic balance (HLB) SPE cartridges for the bioactive substances in biopesticides containing derris extract, and the eluate was analyzed to quantify the rotenone and deguelin by the UPLC. LOQ and recovery rates of rotenone and deguelin were 0.085 and 0.044 mg/L, 95.7 and 93.3%, respectively. The content of rotenone and deguelin in three biopesticides containing derris extract were analyzed by the developed method, the results showed 0.001-0.236 and

LC-MS/MS에 의한 벌꿀 중 잔류 네오마이신의 분석 (Analysis of residual neomycin in honey by LC-MS/MS)

  • 심영은;정지윤;명승운
    • 분석과학
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    • 제22권4호
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    • pp.319-325
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    • 2009
  • 벌꿀 중에 잔류하는 아미노그라이코사이드 항생제인 네오마이신을 효과적으로 분석하는 방법을 개발하고 방법에 대한 유효성 검증을 수행하였다. 0.1M 염산을 사용하여 벌꿀의 pH를 2로 조절한 후 고체상 추출(SPE) 고체상인 양이온교환 카트리지에 적재한 후 염기성 메탄올로 용리하였다. 용리된 추출물은 이온쌍 시약을 사용한 이온쌍 크로마토그래피법으로 분리한 후 LC/(+)ESI-MS/MS의 MRM 방법으로 분석하였다. 정량분석을 위해서 spike 한 $5.0{\sim}250{\mu}g/kg$ 농도 범위에서 검정곡선은 좋은 직선성 ($r^2$ > 0.9951)을 나타내었다. 분석방법의 상대표준편차는 11.5~18.7%이었고 정확도는 bias로 10.9~20.9%이었다. 확립된 분석방법은 벌꿀 중에서 네오마이신의 분석방법으로 유용하게 사용될 수 있을 것이다.