• Title/Summary/Keyword: HPLC/FLD

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Influence of Roasting Conditions on Polycyclic Aromatic Hydrocarbon Contents in Ground Coffee Bean (원두커피의 로스팅 조건이 polycyclic aromatic hydrocarbons 생성에 미치는 영향)

  • Nam, He-Jung;Seo, Il-Won;Shin, Han-Seung
    • Korean Journal of Food Science and Technology
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    • v.41 no.4
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    • pp.362-368
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    • 2009
  • Roasting may lead to the formation of undesired compounds, such as polycyclic aromatic hydrocarbons (PAHs). In this study, green coffee beans were roasted under controlled conditions and the formation of PAHs during the roasting process was monitored. Roasting was performed in a hot air roaster, with an inlet air temperature varying from 150 to $250^{\circ}C$ for 5, 10, and 20 min. The PAH content of the roasted coffee was then evaluated by HPLC-FLD. The levels of total PAHs in Arabica (Colombia, Brazil) and Robusta (India) coffee samples were 1.26-215.07, 1.85-178.14, and 0.18-2.61 ${\mu}g$/kg, respectively.

Analysis of Flumeqnine in Meats (식육 중 항생제 flumequine의 분석)

  • Kuk, Ju-Hee;Ko, Yong-Seok;Kim, Yong-Hoon;Yoon, Chang-Yong;Sun, Nam-Kyu;Kim, Eun-Jung;Seo, Jee-Woo;Park, Ji-Won;Kang, Kil-Jin
    • Korean Journal of Food Science and Technology
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    • v.41 no.1
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    • pp.7-10
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    • 2009
  • An analytical method for the determination of flumequine in meats was developed and validated using high-performance liquid chromatography with fluorescence detection. The samples were mixed with sodium sulfate and extracted with ethyl acetate. After clean-up, the residues were dissolved in mobile phase. The calibration curves showed high linearity ($r^2$=0.9979) within the concentration range of 0.1-1.0 mg/kg. The limit of detection and limit of quantification were validated at 0.005 and 0.017 mg/kg, respectively. The recoveries in fortified meats ranged from 90.8 to 101.1%. The method was then validated in correspondence with the CODEX guidelines for flumequine residue in meats. Herein we monitored 150 samples of meats that were purchased in Korea (Seoul, Busan, Daegu, Daejeon, and Gwangju). Among the tested samples, flumequine was detected in 1 of beef and 1 of pork at levels in the range of 0.048-0.080 mg/kg. Overall, the flumequine residues in the tested samples were within the Maximun residue limit.

Investigation and Risk Characterization on the Contamination Level of Herbal Medicines Without Legal Benzo(a)pyrene Specification (벤조피렌 기준 미설정 한약재의 오염도 조사 및 위해도 결정)

  • Park, Young-Ae;Ko, Suk-Kyung;Cho, Seok-Ju;Hwang, In-Sook;Shin, Gi-Young;Moon, Kwang-Deog
    • Korean Journal of Pharmacognosy
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    • v.52 no.4
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    • pp.219-227
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    • 2021
  • By analysing the benzo(a)pyrene concentration using HPLC-FLD and LC-MS/MS, pollution levels of herbal medicines without permitted benzo(a)pyrene specification were investigated. Average benzo(a)pyrene concentrations were 38.30, 37.46 and 21.22 ㎍/kg for Amomi Tsao-ko Fructus, Mume Fructus and Coptidis Rhizoma, respectively, which are 4 to 7 times higher than maximum permitted benzo(a)pyrene concentration of Rehmanniae Radix Preparata and Rehmanniae Radix, i.e. 5.0 ㎍/kg. Proportion of detected samples exceeding 5.0 ㎍/kg benzo(a)pyrene concentration was 22% for Cimicifugae Rhizoma and Scrophulariae Radix, 44% for Forsythiae Fructus, 67% for Mume Fructus, 100% for Amomi Tsao-ko Fructus and Coptidis Rhizoma, and collectively 29% (36 out of 125 samples) in average. In terms of risk characterization results, human exposure of benzo(a)pyrene were 7.96, 3.49 and 1.61 ng/kg b.w./day and the margin of exposure(MOE) were 1.25 × 104, 2.86 × 104 and 6.20 × 104 for Mume Fructus, Amomi Tsao-ko Fructus and Coptidis Rhizoma, respectively. MOE banding of those herbal medicines was categorized to 'low concern'. However, considering that human exposure of benzo(a)pyrene for food is legislated to 1.4~2.5 ng/kg b.w./day, it was urgent to set up the guideline of benzo(a)pyrene in herbal medicines.

Pesticide Residues Survey and Safety Evaluation for Perilla Leaf & Lettuce on the Garak-dong Agricultural & Marine Products Market (가락동 농수산물도매시장 반입 들깻잎과 상추의 잔류농약 실태 및 안전성 평가)

  • Park, Won-Hee;Hwang, In-Sook;Kim, Eun-Jeong;Cho, Tae-Hee;Hong, Chae-Kyu;Lee, Jae-In;Choi, Su-Jeong;Kim, Jin-A;Lee, Yun-Jeong;Kim, Mi-Sun;Kim, Gi-Hae;Kim, Moo-Sang
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.151-160
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    • 2015
  • This study was conducted to monitor residual pesticides in perilla leaf & lettuce and to assess their risk to human health. The total number of perilla leaf & lettuce were 4,063 and 2,248 respectively and these products were collected at the Garak-dong Agricultural & Marine Products Market sold by auction from 2010 to 2012. Multi-residual analysis of 285 pesticides were performed by GC-ECD, GC-NPD, HPLC-DAD and HPLC-FLD. In perilla leaf, 61 pesticides were detected and detection rate was 20.0%. 28 pesticides were detected in case of lettuce and detection rate was 4.8%. In order to do risk assessment by perilla leaf & lettuce consumption, estimated daily intake of residual pesticides were determined and compared to acceptable daily intake, referring to hazard index (HI values). The range of % HI values of perilla leaf was from 0.000% to 0.049%. The range of % HI values of lettuce was from 0.000% to 0.095%. These results show that the risk caused by pesticide residues in perilla leaf & lettuce intake were very low and these vegetable intake was safe.

Monitoring of Pesticide Residues in Leafy Vegetables Collected from Wholesale and Traditional Markets in Cheongju (청주지역 도매 및 재래시장 유통 엽채류 중 잔류농약 모니터링)

  • Noh, Hyun-Ho;Park, Young-Soon;Kang, Kyung-Won;Paik, Hyo-Kyung;Lee, Kwang-Hun;Lee, Jae-Yun;Yeop, Kyung-Won;Choi, Song-Rim;Kyung, Kee-Sung
    • The Korean Journal of Pesticide Science
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    • v.14 no.4
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    • pp.381-393
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    • 2010
  • In order to monitor the residual characteristics of the pesticides in leafy vegetables selling at wholesale markets and traditional markets in Cheongju, a total of 180 samples of 15 leafy vegetables, such as broccoli, celery, chard, chicory, Chinese vegetable, Chwinamul, crown daisy, Korean cabbage, leek, lettuce, perilla leaves, Shinsuncho, spinach, welsh onion and young radish, were purchased from the wholesale markets and traditional markets in June and August in 2010 and the pesticide residues in them were analyzed by multiresidue analysis method using GLC, HPLC and GC-MSD. Seven pesticides were detected from 12 samples out of total 180 samples collected, representing detection rate was 6.7%. In case of the samples collected from markets in June, four pesticides including tefluthrin were detected from six samples and in case of the samples collected from markets in August, three pesticides including pendimethalin were detected from three samples. The MRL-exceeding rate of pesticides detected from leafy vegetables was 0.6%. The pesticide exceeded its MRL was azoxystrobin detected from crown daisy and many pesticides were not registered to the crops, excepting that azoxystrobin detected from Chwinamul and tefluthrin from leek. Estimated daily intakes (EDIs) of the pesticides detected from leafy vegetables were less than 7% of their acceptable daily intakes (ADIs), representing that residue levels of the pesticides detected were evaluated as safe.

The Analysis and Migration of Bisphenol A Related Compounds from Metal Food Cans (식품용 금속 캔으로부터 비스페놀 A 관련 물질들의 분석 및 이행 연구)

  • Park, Se-Jong;Park, So-Ra;Choi, Jae Chun;Kim, MeeKyung
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.329-335
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    • 2017
  • Analysis method was presented for the simultaneous determination of nine bisphenol A related compounds such as bisphenol A (BPA), phenol, p-tert-butylphenol, bisphenol A diglycidyl ether (BADGE), $BADGE{\cdot}2H_2O$, $BADGE{\cdot}2HCl$, bisphenol F diglycidyl ether (BFDGE), $BFDGE{\cdot}2H_2O$ and $BFDGE{\cdot}2HCl$ migrated from inner coatings of metal food cans by high performance liquid chromatography (HPLC) with fluorescence detection. The method was validated by examining the linearity of calibration curve, the limit of detection (LOD), the limit of quantification (LOQ), recovery and uncertainty. The migration tests of nine BPA related compounds were carried out with four food simulants; deionized water (DW), 4% acetic acid, 50% ethanol and n-heptane. There was not any compound detected in DW, 4% acetic acid and 50% ethanol at $60^{\circ}C$ for 30 min and n-heptane at $25^{\circ}C$ for 60 min. BPA and phenol were migrated into 4% acetic acid and 50% ethanol at $95^{\circ}C$ for 30 min. The concentrations were ranged from 0 to $10.77{\mu}g/L$ of BPA and from 0 to $2.35{\mu}g/L$ of phenol. Canned foodstuffs mostly have long-term shelf life. We investigated migration of nine BPA related compounds according to the variation in storage periods (0~90 days) and temperatures (4, 25 and $60^{\circ}C$). All compounds were not founded during 90 days at $4^{\circ}C$ and $25^{\circ}C$, respectively. However BPA and $BADGE{\cdot}2H_2O$ were founded in DW and 4% acetic acid at $60^{\circ}C$. The migration levels of BPA and $BADGE{\cdot}2H_2O$ were close to the value of LOQ, respectively and did not change significantly as storage period. It was founded from results that the migration of BPA related compounds from metal food cans was controlled to a safe level.

Determination of Polycyclic Aromatic Hydrocarbons in Smoked Food Products (훈연식품 중 polycyclic aromatic hydrocarbons 함량 분석)

  • Seo, Ilwon;Nam, Hejung;Lee, Songyoung;Lee, Kyueun;Shin, Han-Seung
    • Food Engineering Progress
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    • v.13 no.3
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    • pp.195-202
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    • 2009
  • This study was accomplished that analysis of seven polycyclic aromatic hydrocarbons (PAHs) in smoked or nonsmoked processing foods by high performance liquid chromatography (HPLC) with fluorescence detection. The calibration line was constructed with injected different levels of standard concentration. Limit of detection (LOD) and limit of quantification(LOQ) showed higher linearity ($r^{2}$=0.998) reasonably, and recovery exhibited 0.033-0.666 $\mu$g/kg, 0.108-2.217 $\mu$g/kg and 69.31-90.14%, respectively. As a result, the samples using smoked tuna as smoked materials contained seven PAHs with different range from 0.256 to 0.486 $\mu$g/kg. The benzo[a]pyrene, indicator of PAHs, was detected to below the LOQ in two samples. Concentrations of benzo[a]pyrene in three samples were below the 2 $\mu$g/kg which is the limit of regulation. Smoked tuna sauces were detected from 0.321 to 0.552 $\mu$g/kg and not detected in drying powders. PAHs of smoked meat products were ranged from 0.720 to 2.027 $\mu$g/kg and are higher than concentration of tuna smoked samples. PAHs were very low in non-smoked foods including mustard, herb, and roasted meats.

Monitoring of Pesticide Residues and Risk Assessment on Agricultural Products Marketed in the Northern Area of Seoul in 2013 (2013년 서울북부지역 유통농산물의 잔류농약 모니터링 및 위해성 평가)

  • Kim, Nam Hoon;Lee, Jeong Sook;Kim, Ouk Hee;Choi, Young Hee;Han, Sung Hee;Kim, Yun Hee;Kim, Hee Sun;Lee, Sae Ram;Lee, Jeong Mi;Yu, In Sil;Jung, Kwon
    • Journal of Food Hygiene and Safety
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    • v.29 no.3
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    • pp.170-180
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    • 2014
  • The aim of this study was to investigate pesticide residues in 2,877 market vegetables in the northern area of Seoul in 2013. Pesticide residues in the samples were analysed by multiresidue method for 285 pesticides using GC-ECD/NPD and HPLC-DAD/FLD. 385 samples(13.4%) were detected with pesticide residues at or below MRL, and 15 samples(0.5%) were found to detect pesticide residues exceeding MRL. The most frequently detected samples were sedum(63.6%), chamnamul(45.8%), leek(44.5%) and green&red pepper(30.8%). Among the 15 violated samples, leek(5 cases) and welsh onion(4 cases) showed the highest violation rate. A total of 74 samples(18.5%) contained multiple pesticide residues in one vegetable. Procymidone, chlorofenapyr and cypermethrin were the pesticide most frequently found. As a tool of risk assessment through the consumption of pesticide detectable agricultural products, the ratio of estimated daily intake (EDI) to acceptable daily intake (ADI) was calculated into the range of 1.05~28.61%. The results have meant that there was no health risk through dieting commercial agricultural products detected with pesticide residues.

Analysis of PAHs (polycyclic aromatic hydrocarbons) in Ground Coffee Using GC-tandem Mass Spectrometry and Estimation of Daily Dose (GC-tandem mass spectrometry를 이용한 분쇄원두커피 중 PAHs(polycyclic aromatic hydrocarbons) 분석법 연구 및 인체노출량 평가)

  • Jung, So-Young;Park, Ju-Sung;Son, Yeo-Joon;Choi, Su-Jeong;Lee, Yun-Jeong;Kim, Mi-Sun;Park, So-Hyun;Lee, Sang-Me;Chae, Young-Zoo
    • Korean Journal of Food Science and Technology
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    • v.43 no.5
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    • pp.544-552
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    • 2011
  • The purpose of this study was to develop an analytical method for determining 15 polycyclic aromatic hydrocarbons (PAHs) of EU priority using gas chromatography (GC)-tandem mass spectrometry (MS). The PAHs in ground coffee were analyzed after being extracted using methods such as saponification-liquid-liquid extraction, Soxhlet extraction, and solid-liquid extraction. The solid-liquid extraction method showed the greatest repeatability and most efficient reduction of the matrix effect. GC-tandem MS for the quantification of the 15 PAHs showed better resolution and lower limit of detections (LODs) than GC-MS-selected ion monitoring (SIM) and high performance liquid chromatography with fluorescence detector. LODs of this method for the ground coffee types were 0.002-0.1 ${\mu}g/kg$ and limit of quantifications (LOQs) were 0.006-0.2 ${\mu}g/kg$ The recoveries ranged from 52.6 to 93.3%. Forty-six commercial types of ground coffee were analyzed to determine their PAHs contamination levels. PAHs concentration ranged from ND to 5.988 ${\mu}g/kg$. This study was conducted with toxicity equivalence factors, the U.S. EPA recommendation to identify dietary risks for PAHs in different types of coffee. The estimated average daily dose of PAHs was $5.24{\times}10^{-8}$ mg/kg body weight/day.

Monitoring of Pesticide Residues in Floricultural Crops Collected from Floral Farms and Markets in Korea (국내 재배.유통 중인 화훼의 잔류농약 모니터링)

  • Lee, Kyung-Hee;Kim, Seong-Soo;Park, Hong-Ryeol;Ji, Kwang-Yong;Kim, Jong-Geol;Huh, Kun-Yang;Hur, Jang-Hyun
    • The Korean Journal of Pesticide Science
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    • v.13 no.4
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    • pp.216-222
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    • 2009
  • The present study aims to monitor pesticide residues in cut flowers collected from the farms and markets. Cut flowers used in this study included rose, lily and chrysanthemum collected from June to September, 2008. Samples were collected once from farms in Hwasung, Goyang (Gyeonggi-do), Inje (Gangwon-do) and thrice from wholesale market in Namdaemunm, Yangjae and Gangnam (Seoul). Total of 24 pesticides (12 fungicides, 11 pesticides and 1 acaricide) were detected from samples collected from farm and total of 64 pesticides (25 fungicides, 36 pesticides, 1 acaricide and 2 fungicides) were detected from samples collected from wholesale market. The highest detection frequency of pesticide from farm was for carbaryl (15%) and for boscalid, fluacrypyrin, fluquinconazole, methomyl, pyraclostrobin, trifloxystrohin (10%), with overall detection of $0.1-36.99\;mg\;kg^{-1}$. While the highest detection frequency of pesticides from wholesale market was for carbaryl, fluquinoconazole and kresoxim-methyl (18.52%), methomyl (16.6%), and methiocarb and thiacloprid (12.96%) with overall detection amount of $0.1-56.2\;mg\;kg^{-1}$. Higher amount of pesticides were detected in leaves than in flowers. Among the pesticides detected, detection frequency of unregistered pesticides for rose, chrysanthemum and lily was 55%, 60% and 63% collected from farms and 47%, 60% and 89% collected from markets, respectively. These pesticides require registration and further monitoring in floricultural crops.