• Title/Summary/Keyword: HPLC/FLD

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A survey on pesticide residues of imported fruits circulated in Gyeonggido (경기도내 유통 수입과실류의 잔류농약 실태조사)

  • Cho, Yun-Sik;Kang, Jeong-Bok;Kim, Yang-Hee;Jeong, Jin-A;Huh, Jeong-Weon;Lee, So-Hyun;Lim, Young-Sik;Bae, Ho-Jeong;Kang, Heung-Gyu;Lee, Jeong-Hee;Jung, Eun-Sook;Lee, Byoung-Hoon;Park, Yong-Bok;Lee, Jong-Bok
    • The Korean Journal of Pesticide Science
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    • v.16 no.3
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    • pp.195-201
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    • 2012
  • We tested for pesticide residues in 124 samples of 22 different items of imported fruits circulated in Gyeonggido. Total 218 pesticides were analyzed by multi-residue method using gas chromatography/nitrogen phosphorus detector-electron capture detector (GC/NPD-ECD), time of flight/mass spectrometer (TOF/MS), ultra performance liquid chromatography/photo diode array (UPLC/PDA), high performance liquid chromatography/fluorescence detector (HPLC/FLD) and mass spectrometer (LC/MS/MS). The pesticides were detected in 18 fruits samples, ranging 0.003~0.3 mg/kg and no samples had violative residue. The separation test to 14 sample pesticides detected was conducted to monitor the current status of pesticide residues according to the partial characteristic. The pesticides were detected in 14 peels ranging 0.03~1.5 mg/kg and 2 fleshes in less than detection limits. These results indicate that imported fruits are safe when the human takes normally but even the small amount of pesticides is harmful when the human takes it in a prolonged period. Therefore, the pesticide residual amounts of imported friuts should be constantly monitored for food safety.

Monitoring and Risk Assessment of Pesticide Residues in Commercial Environment Friendly Fruits and Fruiting Vegetables (유통 친환경 과실류와 과채류 중 농약잔류 실태조사 및 안전성 평가)

  • Lee, Jae Yun;Noh, Hyun Ho;Park, So Hyun;Lee, Kwang Hun;Park, Hyo Kyoung;Hong, Su Myeong;Kim, Doo Ho;Kyung, Kee Sung
    • The Korean Journal of Pesticide Science
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    • v.16 no.4
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    • pp.308-314
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    • 2012
  • In order to monitor the residual pesticides in environment friendly agricultural commodities, fruits and fruiting vegetables. Twenty-five agricultural commodities were collected twice in May and August 2011 from nine environment friendly agricultural commodities-selling supermarkets and retail stores located in eight major cities in Korea. The number of each agricultural commodity collected, 555 samples in total, was 152 organic agricultural products, 202 pesticide-free agricultural products and 201 low-pesticide agricultural products. Pesticide residues in samples were analyzed by multiresidue method for 245 pesticides using a GC-ECD/NPD and an HPLC-DAD/FLD and the peaks suspected as pesticides were identified with a GC/MSD. As a result of pesticide residue analysis, three pesticides, bifenthrin, EPN and chlorpyrifos, were detected from four samples including apple, representing a detection rate of 0.72%. The residue levels of the four pesticide-detected samples were less than their maximum residue limits (MRLs) but one pesticide EPN detected from pear exceeded its legible criterion of one twentieth MRL. Estimated daily intakes of the pesticides detected from fruits and fruiting vegetables were less than 0.76% of their maximum permissible intake.

Determination of Polycyclic Aromatic Hydrocarbons in Processed Chestnut Products (밤가공품 중 polycyclic aromatic hydrocarbons 함량 분석)

  • Seo, Il-Won;Nam, He-Jung;Kim, Dong-Hyuk;Shin, Han-Seung
    • Korean Journal of Food Science and Technology
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    • v.41 no.3
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    • pp.339-344
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    • 2009
  • Concentrations of polycyclic aromatic hydrocarbon (PAH) in processed chestnut products were determined by HPLC/FLD. The methodology involved procedures of sonication with water, extraction with hexane, and clean-up on a Sep-pak florisil cartridge. The PAH limits of detection (LOD) and limits of quantitation (LOQ) ranged from 0.012 to 0.382 ${mu}g/kg$ and from 0.042 to 1.273 ${mu}g/kg$, respectively. The coefficients of variation for intra- and inter-day assays were 0.02-4.48% and 0.37-9.83%, respectively, and the accuracies were 81.95-125.44% and 79.89-116.53%, respectively. The overall recoveries for eight PAHs spiked into the processed chestnut products ranged from 87.83 to 100.56%. As a result, PAH contents were not detected in the processed chestnut products.

Analysis of ITX from Commercial Carton Packs in Korean Market (국내 유통 종이팩 포장재 중 Isopropylthioxanthone(ITX) 분석)

  • Eom, Mi-Ok;Yoon, Hae-Jung;Choi, Hyun-Cheol;Jeon, Dae-Hoon;Kim, Hyung-Il;Sung, Jun-Hyun;Park, Na-Young;Lee, Eun-Joon;Sung, Duk-Hwa;Lee, Young-Ja
    • Journal of Food Hygiene and Safety
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    • v.22 no.2
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    • pp.88-92
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    • 2007
  • Isopropylthioxanthone(ITX) is used as a photoinitiator In UV-cured inks, triggering the radical polymerization of the acrylic component of such inks and thus causing the liquid ink film to cure. Recently ITX was detected in carton packed food in Italy. In order to cope with risk issues of overseas and acquire monitoring data on ITX, we have established the method using HPLC/FLD for ITX analysis after reviewing parameters of the analytical methods. Limit of detection (LOD) and limit of quantification (LOQ) were 0.02 ppb and 0.1 ppb, and linearity and RSD (%) were 0.9991 and 1.09, respectively. We have investigated ITX levels migrated to food on 87 commercial products packed in carton and ITX was not detected any food. Therefore it is supposed that UV-cured ink containing ITX as photoinitiator is not currently used in printing of carton pack in Korea.

Analysis of Polycyclic Aromatic Hydrocarbon Content in Coffee Beans with Different Preparation Method (전처리 방법에 따른 커피원두 중 polycyclic aromatic hydrocarbons 함량 분석)

  • Nam, He-Jung;Seo, Il-Won;Shin, Han-Seung
    • Korean Journal of Food Science and Technology
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    • v.41 no.2
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    • pp.157-161
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    • 2009
  • This paper proposes an analytical method for determining amounts of polycyclic aromatic hydrocarbons (PAHs; benzo[a]anthracene, chrysene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenzo[a,h]anthracene, benzo[g,h,i] perylene) in coffees beans. Soxhlet extraction and liquid/liquid extraction were tested for the quantification of seven PAHs. Soxhlet extraction was followed by cyclohexane extraction and used a silica cartridge. Liquid/liquid extraction was followed by n-hexane extraction and utilized a florisil cartridge. The extracts were analyzed by HPLC-fluorescence detection (FLD) with a Supelcosil LC-PAH column. The PAH recoveries ranged from 78.68 to 96.28% for the liquid/liquid extraction, and from 67.47 to 84.60% for the Soxhlet extraction.

Anaylsis of ${\gamma}$-aminobutyric Acid (GABA) Content in Germinated Pigmented Rice (발아 유색미의 GABA(${\gamma}$-aminobutyric acid) 함량 분석)

  • An, Mi-Kyoung;Ahn, Jun-Bae;Lee, Sang-Hwa;Lee, Kwang-Geun
    • Korean Journal of Food Science and Technology
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    • v.42 no.5
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    • pp.632-636
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    • 2010
  • The level of ${\gamma}$-aminobutyric acid (GABA) in pigmented rice was quantitatively and qualitatively determined by high pressure liquid chromatography/fluorescence detection (HPLC/FLD). In this study, the recovery rate and limit of detection (LOD) of GABA were 122.4${\pm}$2.4% and 0.23 ${\mu}g/g$, respectively. The geminating pigmented rice samples, which were harvested in Paju, Korea, were soaked in water at $18^{\circ}C$ for 20 hr. After soaking, the samples were germinated at $30^{\circ}C$ for about 24 hr. GABA content was highest (293.0 ${\mu}g/g$) in the germinated red rice. Furthermore, GABA levels in the germinated rice increased significantly by up to 11.1 and 24.7-fold as compared to non-germinated rice and milled rice, respectively. The GABA concentrations of non-germinated rice, with the exception of red rice, were significantly higher than those of milled rice by 7.6-20.6-fold.

Levels of Polycyclic Aromatic Hydrocarbons in Fish, Shellfish and their Processed Products (국내 유통 어패류 및 가공품 중 Polycyclic Aromatic Hydrocarbons 함량)

  • Hu, Soo-Jung;Kim, Mee-Hye;Oh, Nam-Su;Ha, Jin;Choi, Kwang-Sik;Kwon, Ki-Sung
    • Korean Journal of Food Science and Technology
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    • v.37 no.6
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    • pp.866-872
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    • 2005
  • Cocentrations of PAHs [benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h.i)perylene, indeno(1,2,3-c,d)pyrene] in fish (n=120), shellfish(n=50) and their products (n=35) were estimated by saponification and extraction with n-hexane, clean-up on Sep-Pak Florisil Cartridges and HPLC/FLD. Overall recoveries for eight PAHs spiked into samples ranged from 90 to 106%. Mean level of benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene and indeno(1,2,3-c,d)pyrene were not detected, 0.01, 0.04, 0.07, 0.05, 0.004, 0.0008 and 0.06ng/g, respectively, similar to those reported by other countries.

Monitoring of Endocrine Disruptor-suspected Pesticide Residues in Greenhouse Soils and Evaluation of Their Leachability to Groundwater (시설재배 토양 중 내분비계장애 추정농약의 잔류 모니터링 및 지하수 용탈 가능성)

  • Noh, Hyun-Ho;Lee, Kwang-Hun;Lee, Jae-Yun;Park, Hyo-Kyung;Lee, Eun-Young;Hong, Su-Myung;Park, Young-Soon;Kyung, Kee-Sung
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.441-452
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    • 2011
  • This study was carried out to survey the residual characteristics of endocrine disruptor (ED)-suspected pesticides in greenhouse soils and assess their leachabilites to groundwater. Greenhouse soils were collected from 40 sites of greenhouse in 2008 in Korea. Sixteen ED-suspected pesticides which had been using in Korea, such as alachlor, benomyl, carbaryl, cypermethrin, 2,4-D, dicofol, endosulfan, fenvalerate, malathion, mancozeb, metribuzin, metiram, methomyl, parathion, trifluralin, and vinclozolin, in the soils, were analyzed by chromatographic methods using GLC-ECD and HPLC-DAD/FLD. Limits of detection (LODs) of the test pesticides ranged from 0.0004 to 0.005 mg/kg. Recoveries of the target pesticides from soil ranged from 72.69 to 115.28%. Four pesticides including cypermethrin were detected in the range of from 0.001 to 2.019 mg/kg, representing that their detection rate from greenhouse soils was 37.5%. The highest detection rate was observed from endosulfan which was detected from 16 site soils of the total samples, indicating that endosulfan is persistent in soil because of its very low mobility and high adsorption characteristics in soil. Based on the groundwater ubiquity scores (GUSs) of the pesticides detected from greenhouse soils, most of them have little possibilities of groundwater contamination except the fungicide vinclozolin with some leaching potential because of high water solubility and very low soil adsorption property.

Monitoring on Benzo(a)pyrene Content in Oriental medicine (유통 한약재 중 벤조피렌 함유량에 관한 모니터링)

  • Lee, Mi-Yeong;Jung, Sang-Mi;Lee, Gye-Won
    • Journal of Digital Convergence
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    • v.10 no.7
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    • pp.201-206
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    • 2012
  • Benzo(a)pyrene is a polycyclic aromatic hydrocarbons (PAHs) whose metabolites are mutagenic and highly carcinogenic and is listed as a Group 1 carcinogen by the IARC. It has been found at variable concentrations in several foods and is associated with several factors during the process including contaminated raw materials, exposure of environment, and procedure of process or cooking. In this study, benzo(a)pyrene in 45 oriental medicines were determined by HPLC/FLD. The calibration curves of benzo(a)pyrene was linear over the concentration range of 0.5~40 ng/mL with correlation coefficient of above 0.999. The limit of detection (LOD) and limit of quantitation (LOQ) of benzo(a)pyrene were 0.04 and 0.10 ${\mu}g/kg$. Benzo(a)pyrene in 3 samples out of 45 samples was not detected. The level of benzo(a)pyrene in 26 (57.7%), 8 (17.8%) and 7 (15.6%) samples was 0.1~0.5, 0.5~1.0 and 1.0~5.0 ${\mu}g/kg$, respectively. Especially, content of benzo(a)pyrene in Coptis Rhizome is the highest (5.97 ${\mu}g/kg$). In conclusion, these results suggest that could be applied to fundamental study and guideline on drying condition to decrease content of benzo(a)pyrene in oriental medicine.

Studies on the Analysis of Benzo(a)pyrene and Its Metabolites on Biological Samples by Using High Performance Liquid Chromatography/Fluorescence Detection and Gas Chromatography/Mass Spectrometry

  • Lee, Won;Shin, Hye-Seung;Hong, Jee-Eun;Pyo, Hee-Soo;Kim, Yun-Je
    • Bulletin of the Korean Chemical Society
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    • v.24 no.5
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    • pp.559-565
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    • 2003
  • An analytical method the determination of benzo(a)pyrene (BaP) and its hydroxylated metabolites, 1-hydroxybenzo(a)pyrene (1-OHBaP), 3-hydroxybenzo(a)pyrene (3-OHBaP), benzo(a)pyrene-4,5-dihydrodiol (4,5-diolBaP) and benzo(a)pyrene-7,8-dihydrodiol (7,8-diolBaP), in rat urine and plasma has been developed by HPLC/FLD and GC/MS. The derivatization with alkyl iodide was employed to improve the resolution and the detection of two mono hydroxylated metabolites, 1-OHBaP and 3-OHBaP, in LC and GC. BaP and its four metabolites in spiked urine were successfully separated by gradient elution on reverse phase ODS $C_{18}$ column (4.6 mm I.D., 100 mm length, particle size 5 ㎛) using a binary mixture of MeOH/H₂O (85/15, v/v) as mobile phase after ethylation at 90 ℃ for 10 min. The extraction recoveries of BaP and its metabolites in spiked samples with liquid-liquid extraction, which was better than solid phase extraction, were in the range of 90.3- 101.6% in n-hexane for urine and 95.7-106.3% in acetone for plasma, respectively. The calibration curves has shown good linearity with the correlation coefficients (R²) varying from 0.992 to 1.000 for urine and from 0.996 to 1.000 for plasma, respectively. The detection limits of all analytes were obtained in the range of 0.01-0.1 ng/mL for urine and 0.1-0.4 ng/mL for plasma, respectively. The metabolites of BaP were excreted as mono hydroxy and dihydrodiol forms after intraperitoneal injection of 20 mg/kg of BaP to rats. The total amounts of BaP and four metabolites excreted in dosed rat urine were 3.79 ng over the 0-96 hr period from adminstration and the excretional recovery was less than 0.065% of the injection amounts of BaP. The proposed method was successfully applied to the determination of BaP and its hydroxylated metabolites in rat urine and plasma for the pharmacokinetic studies.