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Analysis of 1,4-Dioxane and Chlorohydrins in Food Additives by Purge & Trap GC (퍼지앤트랩-기체크로마토그래피(PT-GC)를 이용한 식품첨가물 중 1,4-디옥산 및 클로로히드린류 분석)

  • 조태용;신영민;반경녀;오세동;이창희;이영자;문병우
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.32 no.7
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    • pp.965-970
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    • 2003
  • This study has been performed to develope a method for the simultaneous determination of 1,4-dioxane (DOX), epichlorohydrin (EPC), propylene chlorohydrin (PCH), ethylene chlorohydrin (ECH) and 1,3-dichloro-2-pro-panol (DCP) in polysorbates, chloline chloride, choline bitartrate, modified starch and spices by purge and trapgas chromatography. Experimental design was used to select a suitable trap by measuring the limit of detection (LOD) and to investigate the effect of temperature and salt of extraction, and the percentage of recovery in various matrix. The LOD of DOX, EPC, PCH, ECH and DCP were 1.38μg, 0.23μg, 3.30μg, 3.97μg, 20.43μg respectively, by means of using Vorcarb 3000 trap with 50C sample sparger. Excluding EPC, the recoveries of target compounds were above 90% in all matrix. Target compounds in polysorbates (17), choline chloride (5), choline bitartrate (5), modified starch (8) and spices (25) were not detected. But 2.5 ppm of DOX was detected in Tween 80.

Persistent Organic Pollutants (POPs) Residues in Greenhouse Soil and Strawberry Organochlorine Pesticides (딸기 시설재배지 토양 및 농산물 중 잔류성유기오염물질(POPs)의 잔류량 - 유기염소계 농약)

  • Lim, Sung-Jin;Oh, Young-Tak;Jo, You-Sung;Ro, Jin-Ho;Choi, Geun-Hyoung;Yang, Ji-Yeon;Park, Byung-Jun
    • Korean Journal of Environmental Agriculture
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    • v.35 no.1
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    • pp.6-14
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    • 2016
  • BACKGROUND: Residual organochlorine pesticides (OCPs) are chemical substances that persist in the environment, bioaccumulate through the food web, and pose a risk of causing adverse effect to human health and the environment. They were designated as persistent organic pollutants (POPs) by Stockholm Convention. Greenhouse strawberry is economic crop in agriculture, and its cultivation area and yield has been increased. Therefore, we tried to investigate the POPs residue in greenhouse soil and strawberry.METHODS AND RESULTS: Extraction and clean-up method for the quantitative analysis of OCPs was developed and validated by gas chromatography (GC) with electron capture detector (ECD). The clean-up method was established using the modified quick, easy, cheap, effective, rugged, and safe(QuEChERS) method for OCPs in soil and strawberry. Limit of quantitation (LOQ) and recovery rates of OCPs in greenhouse soil and strawberry were 0.9-6.0 and 0.6-0.9 μg/kg, 74.4-115.6 and 75.6-88.4%, respectively. The precision was reliable sincerelative standard deviation (RSD) percentage (0.5-3.7 and 2.9-5.2%) was below 20, which was the normal percent value. The residue of OCPs in greenhouse soil was analyzed by the developed method, and dieldrin, β-endosulfan and endosulfan sulfate were detected at 1.6-23, 2.2-28.4 and 1.8-118.6 μg/kg, respectively. Those in strawberry were not detected in all samples.CONCLUSION: Dieldrin, β-endosulfan and endosulfan sulfate in a part of investigated greenhouse soil were detected. But those were not detected in investigated greenhouse strawberry. These results showed that the residue in greenhouse soil were lower level than bioaccumulation occurring.

Analysis of sorbic acid in tea-drink using isotope dilution liquid chromatography tandem mass spectrometry (ID-LC/MS/MS) (동위원소희석 액체 크로마토그래피-질량분석법을 이용한 차음료 중의 소르빈산의 분석)

  • Ahn, Seong-Hee;Lee, In-Sun;Kim, Byung-Joo
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.25-32
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    • 2012
  • Isotope dilution mass spectrometry (ID-MS) based on liquid chromatography tandem mass spectrometry (LC/MS/MS) was developed for the accurate determination of sorbic acid in tea-drink. An isotope analogue of sorbic acid, 13C2-sorbic acid, was obtained by custom synthesis. MS was operated in the negative mode with selected reaction monitoring (SRM) mode of [MH] [MCO2H] channel at m/z 111 67 for sorbic acid and at m/z 113 68 for its isotope analogue. Chromatographic separation was accomplished with a C18 column and an isocratic mobile phase of 55% of 50 mM ammonium acetate (pH 4.5) and 45% of methanol. Homogeneous reference materials were prepared for validation of this method, including repeatability and reproducibility tests, by fortifying tea-drink with sorbic acid in our laboratory. Repeatability and reproducibility studies showed that the ID-LC/MS method is a reliable and reproducible method which provides less than 3.8% of relative standard deviation (RSD) for the analysis of sorbic acid.

Quantitative Determination of Caffeine of Green Tea Seed Ethanol Extract on Anti-obesity in C57BL/6 Mice Fed a High-fat Diet and 3T3-L1 Cells (녹차씨 주정추출물의 카페인 함량 평가와 고지방식이 비만유도 C57BL/6 마우스와 3T3-L1 지방전구세포의 항비만효과)

  • Jung, Myung-A;Lee, Hyunmi;Oh, Dool-Ri;Kim, Yu jin;Bae, Dong Hyuck;Oh, Kyo-nyeo;Shin, Heechan;Kim, Sunoh
    • Journal of Physiology & Pathology in Korean Medicine
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    • v.30 no.2
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    • pp.88-94
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    • 2016
  • The study was carried out to examine the anti-obesity effects of 40% ethanol extract from green tea seed (GS) and quantitative determination of caffeine as its major compound. The specificity was satisfied with retention time and UV spectrum by analysis of caffeine using HPLC and comparison with standard compound. It showed a high linearity in the calibration curve with a coefficient of correlation (R2) of 0.9974. The amount of caffeine in GS was about 4.649 mg/g (0.465%) in the three times analysis, and relative standard deviation (RSD) was less than 0.452% by the validated method. The anti-obesity effects of GS were evaluated by using Oil Red O staining in 3T3-L1 adipocytes and body weight, visceral fat and lipid profiles in high fat diet (HFD)-induced C57BL/6 obese mice. Our results indicated that treatment with GS dose-dependently decreased lipid accumulation contents (p<0.001). Moreover, after oral administration for 30 days feeding with HFD-induced obses mice, GS (100 and 300 mg/kg/day) produced a significant decrease in serum total cholesterol (TC), glutamic oxaloacetic transaminase (GOT), glutamic pyruvic transaminase (GPT) and visceral fat. Thus, the result of this study indicate that the GS may be a useful resource for the management of obesity.

A Survey of Zearalenone in Beans Using High Performance Liquid Chromatography-Fluorescence Detector (HPLC-FLD) and Ultra Performance Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS) (HPLC-FLD 및 LC-MS/MS에 의한 두류 중 제랄레논 오염실태 조사)

  • Jang, Mi-Ran;Lee, Chang-Hui;Lee, Hyo-Jeong;Kim, Ji-Yeon;Son, Sang-Hyeok;Sin, Chun-Sik;Kim, So-Hui;Kim, Dae-Byeong
    • Korean Journal of Food Science and Technology
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    • v.40 no.3
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    • pp.354-359
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    • 2008
  • A survey for zearalenone contamination was conducted on 27 soy bean samples, 27 red bean samples, 16 black bean samples, 19 seoritae samples, 14 seomoktae samples, for a total of 127 commercial Korean samples. Zearalenone was quantified by the immunoaffinity column clean-up method with high performance liquid chromatography-fluorescence detection (HPLC-FLD), and was confirmed by liquid chromatography tandem mass spectrometry(LC-MS/MS). The limits of detection and quantification were 2.0μg/kg and 6.0μg/kg, respectively. The recovery in the beans ranged from 82.2 to 98.4%. According to HPLC-FLD, zearalenone was detected in 13 samples (10.2% incidence), including 1 soybean and 12 red bean samples. The zearalenone contamination levels were in the range of 8.0138.98μg/kg. Finally, LC-MS/MS analysis was conducted in the contaminated samples to verify the results of HPLC-FLD. The LC-MS/MS results confirmed the presence of zearalenone in all 13 samples. The contamination level was lower than that of EU, which is below 100μg/kg for raw grains.

Determination of Amitrole in Water Samples by Evaporation and GC/MS (증발법과 GC/MS를 이용한 수질 시료 중의 Amitrole의 분석법 연구)

  • Yoon, So Hee;Hong, Ji Eun;Pyo, Hee Soo;Park, Song Ja
    • Analytical Science and Technology
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    • v.16 no.6
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    • pp.483-487
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    • 2003
  • Amitrole is well-known as a non-selective herbicide and it is able to cause contamination of driking water as well as pollution of ground water and surface water. However, it is difficult to extract from water because it has a high solubility for water whereas a low solubility for general organic solvents. This method is described for the determination of amitrole in water samples by GC/MS. After evaporation of 10 mL water sample by a vacuum evaporator, amitrole was derivatized with isobutyl chloroformate (iso-BCF) on room temperature for 15~20 min. As a result, the sensitivity for GCfMS was improved as N-isobutoxycarbonyl amitrole derivative was formed. The linearity of the calibration curve showed good as 0.997. The recoveries were obtained more than 94.9% and relative standard deviations were less than 2.8% at 1.0μg/L, 10.0μg/L and 100.0μg/L. The limit of detection showed 0.1μg/L with a signal-to-noise ratio (S/N) of 3.

Analysis of didecydimethylammonium chloride (DDAC) aerosol in inhalation chamber (흡입챔버 내 didecyldimethylammonium chloride(DDAC) 에어로졸의 분석)

  • Yang, Jeong-Sun;Choi, Sung-Bong;Park, Sang-Yong;Lee, Sung-Bae
    • Analytical Science and Technology
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    • v.25 no.5
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    • pp.307-312
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    • 2012
  • To perform inhalation toxicity test by using experiment animals, we set up an analytical method to monitor didecyldimethylammonium chloride (DDAC) in aerosol nebulized into inhalation chambers by ion chromatography. DDAC was adsorbed by XAD-2 resin and analyzed with conductivity detector. Recovery of DDAC desorbed by acetonitrile from XAD adsorbent was 87.8%. The method detection limit (MDL) and the limit of quantitation (LOQ) were 2.97 μg/m3 and 8.92 μg/m3, respectively. Repeatability was calculated as RSD 7.8% in the range of 0~20 μg/mL. Time needed to analyze a sample was less than 5 minutes. Therefore, the analysis of DDAC by ion chromatography was practically useful in monitoring DDAC in inhalation chambers with rapidity and sensitivity manner to perform inhalation toxicity test using experimental animals.

Development of Analytical Method for Picoxystrobin in Agricultural Commodities Using GC/ECD and GC/MS (GC/ECD와 GC/MS를 이용한 농산물 중 Picoxystrobin의 분석법 개발)

  • Kwon, Hye-Young;Kim, Chan-Sup;Park, Byung-Jun;Kim, Il-Hwan;Hong, Su-Myeong;Son, Kyung-Ae;Jin, Yong-Duk;Lee, Je-Bong;Im, Geon-Jae;Kim, Doo-Ho
    • Korean Journal of Environmental Agriculture
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    • v.31 no.2
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    • pp.146-151
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    • 2012
  • BACKGROUND: This study was conducted to develop analytical method for picoxystrobin in agricultural commodities using GC/ECD and GC/MS. METHODS AND RESULTS: Each steps of analytical method were optimized for determining picoxystrobin residues in various agricultural commodities. The developed methods include acetone extraction, n-hexane/saline water partition and florisil column chromatography for analysis of all samples (apple, potato, green pepper, hulled rice and soybean), and in addition to these steps, solid phase extraction (SPE) was used for analysis of green pepper and n-hexane/acetonitrile partition was used for analysis of hulled rice and soybean. The instrumental conditions were tested for quantitation in GC/ECD and for confirmation in GC/MS. Recovery was in the range of 86~109% with RSD 10.2% and the quantitation limits (LOQ) of method were 0.025 mg/kg in all agricultural commodities. CONCLUSION: The result showed that the developed method can be used to determine picoxystrobin residue in agricultural commodities.

Quantitative Determination of Phenol in Water Using GC-MS after Liquid-Liquid Extraction and Acetylation (액-액 추출과 아세틸화 후 GC-MS를 이용한 물 중 phenol의 분석)

  • Park, Sunyoung;Kim, Yunjeong;Jung, Sungjin;Kim, Hekap
    • Korean Journal of Environmental Agriculture
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    • v.36 no.1
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    • pp.63-66
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    • 2017
  • BACKGROUND: The phenol concentrations in water samples were determined using gas chromatography after derivatization of the analyte to phenyl acetate followed by extraction using a large volume of solvent. However, this procedure requires an additional purification step and is not analytically efficient. METHODS AND RESULTS: In this study, phenol was first extracted from an acidified water sample using ethyl acetate and then acetylated using acetic anhydride in the presence of a small amount of water and K2CO3. The derivative was extracted using 1mL of n-butyl acetate. One microliter of the extract was analyzed by GC-MS without further purification. The calibration curve showed good linearity with the r2 value of 0.9968. The method detection limit and the limit of quantitation were estimated to be 0.18μg/L and 0.56μg/L, respectively. Repeatability (RSD, n=3) and recovery (n=3) were 9.1%-4.3% and 90.6%-110.5%, respectively. The concentrations of phenol in a few samples of stream water were distributed in the range of 2.517.51μg/L. CONCLUSION: This method is simpler and faster to implement than those currently utilized and shows high analytical reliability. It can be applied to the quantitative determination of phenol concentrations in surface water and groundwater samples.

Polycyclic Aromatic Hydrocarbons in Agricultural Waterways in Gyeonggi and Gangwon Provinces, Korea (경기 및 강원지역 농업용수 중 PAHs의 모니터링 연구)

  • Kim, Leesun;Park, Byung-Jun;Lee, Sung-Eun
    • Korean Journal of Environmental Biology
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    • v.34 no.3
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    • pp.216-221
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    • 2016
  • Level and distribution of fourteen polycyclic aromatic hydrocarbons (PAHs) in the agricultural water samples collected in the waterways located in Gyeonggi and Gangwon, Korea were determined for monitoring and risk assessment. A simplified, fast but effective extraction and clean-up methods combined with gas chromatography tandem mass spectrometry (GC-MS/MS) was employed to measure the concentration of the target compounds. The extraction of the analytes of interest in water sample (10 mL) was performed with acetonitrile (10 mL) and the salt. To purify the target PAHs, the clean-up procedure was employed with 2 mL tubes of dispersive solid phase extraction. The optimized method was validated with recoveries, method detection limit (MDL), accuracy and precision. Good recoveries for each PAHs at 10 and 25μgL1 were achieved (60 to 110%, with RSD <20%) with linearity (>0.99). MDL for all the analytes was achieved with 0.2μgL1. GC-MS/MS results showed that concentration of phenanthrene in the water samples from Gyeonggi (20 sites) ranged from 0.82 to 2.56μgL1 and from Gangwon (15 sites) ranged from 0.83 to 1.62μgL1. Other PAHs were not found in the water samples but the continuous monitoring for these areas were required.