• Title/Summary/Keyword: extraction and clean-up methods

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Nucleotide Analysis in Korean Dairy Products Using High- Performance Liquid Chromatography with Diode Array Detector

  • Won, Jong-Eun;Bang, Han-Yeol;Kwak, Byung-Man;Park, Jong-Su;Kim, Gui-Ran;Kwon, Joong-Ho
    • Food Science of Animal Resources
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    • v.39 no.1
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    • pp.93-101
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    • 2019
  • Nucleotides play important roles in numerous intracellular biochemical processes and are used in infant formulas and other dairy products. However, domestic analytical methods for assessing nucleotide content in products have not yet been established, and therefore, methods for determining nucleotide content are urgently required. A rapid and simple analytical method for determining the content of five types of nucleotides in dairy products was improved using solid phase extraction clean-up and high-performance liquid chromatography with diode array detector. The extraction solvent used in the AOAC method was not well dissolved and was changed to hydrophilic EDTA-Na. In addition, the results obtained using the isocratic elution method and a single wavelength were similar to those obtained using the AOAC method, and the time taken for analysis was shortened from 40 min to 25 min. The process of method validation revealed the following parameters: accuracy (84.69%-102.72%), precision (1.51%-6.82%), linearity (0.999), and limit of detection (cytidine 5'-monophosphate, 0.09 mg/L; uridine 5'-monophosphate, 0.11 mg/L; adenosine 5'-monophosphate, 0.12 mg/L; guanosine 5'-monophosphate, 0.11 mg/L; and inosine 5'-monophosphate, 0.14 mg/L). The method was also used to determine the nucleotide concentration in 25 samples (infant formulas, 1.99-29.39 mg/100 g; and cow milk, 0.28-0.83 mg/100 g). The newly improved method was appropriate for analyzing nucleotides in infant formulas and other dairy products faster when compared to conventional methods.

Status of Soil Remediation and Technology Development in Korea (국내 오염토양 복원 현황과 기술 동향)

  • Yang, Ji-Won;Lee, You-Jin
    • Korean Chemical Engineering Research
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    • v.45 no.4
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    • pp.311-318
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    • 2007
  • Soil contamination in Korea has been accelerated every year. Because of their persistence and cumulative tendency in the environment, soil contaminants have potential long-term environmental and health concerns and it is estimated to cost enormous expense for clean-up. Korea government has legislated the law on conservation of soil environment in mid 1990s, and managed and treated hazardous wastes in contaminated sites as a remediation policy since then. Soil remediation technologies are classified into in-situ/ex-situ or biological/physico-chemical/thermal processes according to applied places or treatment methods, respectively. In Korea, clean-up of polluted sites has been mostly carried out at military areas, railroad-related sites and small-scale oil spilt sites. For these cases, in-situ remediation technologies such as soil vapor extraction (SVE) and bioventing were mainly used. In recent days, an environmental-friendly soil remediation emerged as a new concept - for example, a new soil remediation process using nanotechnology or molecular biological study and an integrated process which can overcome the limitation of individual process. To have better applicability of remediation technologies, comprehensive understandings about the pollutants and soil characteristics and the suitable techniques are required to be investigated. Above all, development of environmental technologies based on the sustainability accompanied by public attention can improve soil environment in Korea.

Pesticide Multiresidues Analysis of Environmental-friendly Agricultural Soils by the Complex Cleanup Method of Accelerated Solvent Extraction (ASE) and Solid Phase Extraction (SPE) (ASE 및 SPE 복합정제법을 이용한 친환경농업토양의 다성분잔류농약 분석)

  • Moo, Kyung-Mi;Park, Jin-Woo;Lee, Young-Guen;Choi, Young-Whan
    • Journal of agriculture & life science
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    • v.45 no.5
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    • pp.73-80
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    • 2011
  • Fifty substances of pesticide were selected for analysis through the historical investigation of pesticides detected from environmental-friendly agricultural soil, and the environmental-friendly agricultural soils in Gyeongnam area were collected and then were accepted Anve (accelerated solvent extraction) and SPve (solid-phase extraction) as multiresidue extraction and clean up methods suitable to the soils. The pesticide residues were analyzed by using GC/vCD/NPD, HPLC/UV/FL, GC/MSD, or HPLC/MSD. 50 kinds of pesticides for the soils were an average of 95.5% from retrieval ratio of the 72 to 118% range, and the average of 3.0% for CV (%). Among 40 samples of soil, 20 components were detected from pesticide residues of 21 samples, and average amounts detected for these components were 0.035 for endosulfan, 0.043 for ethoprophos, 0.020 for chlorpyrifos, 0.023 for chlorfenapyr, 0.047 for flufenoxuron, 0.070 for fenvalerate, 0.266 for cypermethrin, 0.016 for lufenuron, 0.022 for bifenthrin, 0.025 for fenobucarb/BPMC, 0.043 for difenoconazole, 0.059 for fenarimol, 0.020 for kresoxim-methyl, 0.026 for tetraconazole, 0.039 for isoprothiolane, 0.017 for iprobenfos, 0.014 for nolrimol, 0.156 for fluquinconazole, 0.047 for tebuconazole, and 0.045 mg/kg for oxadiazon. Therefore it is infered that the establishment of pesticide residues limit for environmental-friendly agricultural soil is needed as soon as possible.

Sample Pretreatment and HRGC/HRMS Analysis for Determination of Dioxins in Environmental Samples (환경시료 중 다이옥신류의 정량을 위한 시료전처리방법의 개선 및 고분해능 GC/MS 분석에 관한 연구 Ⅰ)

  • Kim, Jin Yeong;Jang, Yun Seok;Lee, Dae Un
    • Journal of the Korean Chemical Society
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    • v.38 no.11
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    • pp.819-826
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    • 1994
  • This study described a simple, rapid and cost effective analytical technique for the ultra-trace analysis of dioxins in environmental samples. Liquid-Liquid extraction methods were used for the initial extraction and enrichment of the analyte. Subsequent clean-up procedures were achieved by using strong cation exchanger, silica and Florisil cartridges. Extracts were analysed by HRGC/HRMS-SIM. The efficiency of these analytical methods was tested by recovery and selectivity for elimination of interferences such as phenols, pesticides and PCBs in each step. The mean recovery of 1,2,3,4-TCDD spiked at 10 ppt in sea water was about 92(${\pm}$1.6)%. This analytical method was applied to Kwangyang sea water and 4.5pg/L of 2,3,7,8-TCDD was determined.

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Evaluation of Chemical Analysis Method and Determination of Polycyclic Aromatic Hydrocarbons Content from Seafood and Dairy Products

  • Lee, So-Young;Lee, Jee-Yeon;Shin, Han-Seung
    • Toxicological Research
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    • v.31 no.3
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    • pp.265-271
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    • 2015
  • This study was carried out to investigate contents of 8 polycyclic aromatic hydrocarbons (PAHs) from frequently consumed seafood and dairy products and to evaluate their chemical analysis methods. Samples were collected from markets of 9 cities in Korea chosen as the population reference and evaluated. The methodology involved saponification, extraction with n-hexane, clean-up on Sep-Pak silica cartridges and gas chromatograph-mass spectrometry analysis. Validation proceeded on 2 matrices. Recoveries for 8 PAHs ranged from 86.87 to 103.57%. The limit of detection (LOD) 8 PAHs was $0.04{\sim}0.20{\mu}g/kg$, and limit of quantification (LOQ) of 8 PAHs was $0.12{\sim}0.60{\mu}g/kg$. The mean concentration of benzo[a]pyrene (BaP) was $0.34{\mu}g/kg$ from seafood and $0.34{\mu}g/kg$ from dairy products. The total PAHs concentration was $1.06{\mu}g/kg$ in seafood and $1.52{\mu}g/kg$ in dairy products.

Investigation of Domoic acid in Shellfish Collected from Korean Fish Retail Outlets

  • Choi, Kyu-Duck;Lee, Jong-Soo;Lee, Jong-Ok;Oh, Keum-Soon;Shin, Il-Shik
    • Food Science and Biotechnology
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    • v.18 no.4
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    • pp.842-848
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    • 2009
  • The purpose of this study was to determine the extent of domoic acid (DA) a potent neurotoxin, responsible for the syndrome amnesic shellfish poisoning (ASP) contamination of various species of bivalve shellfish purchased from fish market in Korea and the implications for food safety. Liquid chromatography (LC) methods were applied to quantify DA in shellfish after sample clean-up using solid-phase extraction (SPE) with strong anion exchange (SAX) cartridges. Toxin detection was achieved using photodiode array ultraviolet (LC-UV) and electrospray ionization-mass (LC-ESI-MS). DA was identified in 4 bivalve shellfishes of 872 shellfishes collected from March, 2006 to October, 2007 in Korea. DA amount of 3 surf clams (Mactra veneriformis) collected at Seoul, Daejeon, and Daegu were 4.13, 1.99, and 1.94 mg/kg, respectively. DA amount of 1 pink butterfly shell (Peronidia venulosa) collected at Seoul was 3.02 mg DA/kg. The amounts of DA that were present in 4 bivalve shellfishes were within EU guideline limits for sale of shellfish (20 mg DA/kg).

An Improved Method for Multiresidue Analysis of Pesticides in Lettuce, Chinese Cabbage and Green Pepper by Gas Chromatography

  • Hong, Yong-Soon;Park, Hee-Won;Choi, Hoon;Moon, Joon-Kwan;Kim, Min-Jeong;Kim, Jang-Eok;Lee, Young-Deuk;Oh, Chang-Hwan;Kim, Jeong-Han
    • Korean Journal of Environmental Agriculture
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    • v.23 no.3
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    • pp.158-169
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    • 2004
  • For the improvement of gas chromatographic analysis of multiple pesticide residues in green pepper, lettuce and Chinese cabbage, multiresidue test mixtures (MRTMs) of 10 groups (ECD 5 groups and NPD 5 groups) and a recovery test mixture (RTM) of 18 compounds (11 compounds for ECD and 7 compounds for NPD) were established based on retention time and response to relevant detectors. A new extraction solvent (acetone: acetonitrile=1 : 9) and a clean up eluent (hexane: dichloromethane : acetonitile = 50 : 48.5 : 1.5) for solid-phase extraction (SPE) cartridge were selected to test two types of multiresidue methods (MRM I and MRM II). MRM II provided high recovery better than MRM I when RTM was tested Recovery experiment with MRTMs which was conducted using MRM II resulted in that more than seventy percents of compounds were recovered in the range of $50{\sim}140%$, while 9% of compounds were over 140% of recovery and only $7{\sim}8$ compounds failed to detect. MRM II, an improved method, could be employed for screening residues of 190 pesticides in those vegetables.

High Performance Liquid Chromatographic Method for Determination of Metazosulfuron Residue in Representative Crops

  • Lee, Hyeri;Kim, Eunhye;Lee, Young Deuk;Kim, Jeong-Han
    • Korean Journal of Environmental Agriculture
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    • v.32 no.2
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    • pp.128-135
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    • 2013
  • BACKGROUND: This study was performed to develop a single residue analytical method for new herbicide metazosulfuron in crops. METHODS AND RESULTS: Brown rice, apple, mandarin, Kimchi cabbage and soybean were selected as representative crops, and clean-up system, partition solvent and extraction solvent were optimized. Instrumental limit of quantitation (ILOQ), linearity of calibration curve and method limit of quantitation (MLOQ) were determined based on the chromatography and whole procedures. For recovery tests, brown rice, apple, mandarin, Kimchi cabbage and soybean samples were macerated and fortified with metazosulfuron standard solution at three levels (MLOQ, 10 MLOQ and 100 MLOQ). And then those were extracted with acetonitrile, concentrated, and partitioned with ethyl acetate. Then the extracts were concentrated again and cleaned-up through $NH_2$ (aminopropyl) SPE cartridge with acetone : dichloromethane (1% acetic acid) (20 : 80, v/v) before concentration and analysis with HPLC. CONCLUSION(S): ILOQ of metazosulfuron was 2 ng (S/N${\geq}$10) and good linearity was achieved between 0.05 and 12.5 mg/Kg of metazosulfuron standard solutions, with coefficients of determination of 0.9999. MLOQ was 0.02 mg/Kg. Good recoveries from 74.1 to 116.9% with coefficients of variation (C.V.) of less than 10% were obtained, regardless of sample type, which satisfies the criteria of Korea Food and Drug Administration (KFDA). Those results were reconfirmed with LC-MS (SIM). The method established in this study is simple, economic and efficient to be applied to most of crops as an official and general method for residue analysis of metazosulfuron.

Determination of Vitamin B12 (Cyanocobalamin) in Fortified Foods by HPLC

  • Park, Youn-Ju;Jang, Jae-Hee;Park, Hye-Kyung;Koo, Yong-Eui;Hwang, In-Kyeong;Kim, Dai-Byung
    • Preventive Nutrition and Food Science
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    • v.8 no.4
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    • pp.301-305
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    • 2003
  • This study was conducted to develop an HPLC method for determining vitamin B$_{12}$ in fortified foods which has typically been determined by microbiological assays according to AOAC and Korean Food Code approved methods. Vitamin B$_{12}$ (cyanocobalamin) was determined by reversed-phase HPLC with a triple column and UV/VIS dectector (550 nm) using the column switching technique after extraction with 5 mM potassium phosphate solution by sonication without a clean-up procedure. The recovery of spiked samples and limit of detection (LOD) by HPLC were 78.6 ∼107.5 % and 2 ppb ($\mu\textrm{g}$/kg), respectively. The LOD of the microbiological assay (MBA) was much lower than that of HPLC. The concentrations of vitamin B$_{12}$ analyzed in all tested samples (n=12) confirmed compliance with declared label claims. The range of recovery ratio by the HPLC method when compared to the microbiological assay was 76.2 ∼140.0 %. There was not significant difference between the HPLC and MBA methods (p < 0.01) with r=0.9791 and linear regression y=0.9923x-0.04. The HPLC method for determining vitamin B$_{12}$ using the column-switching technique appears to be suitable for determining vitamin B$_{12}$ concentrations above 1 $\mu\textrm{g}$/100 g in fortified foods.ied foods.

Study on New Extraction Method of Microcystins from Cyanobacteria (남조류로부터 마이크로시스틴을 추출하는 새로운 추출법 연구)

  • Pyo, Dong Jin;Shin, Hyun Du
    • Journal of the Korean Chemical Society
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    • v.45 no.2
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    • pp.149-155
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    • 2001
  • A new analytical method of cyanobacterial toxins, i, e, microcysins was deveeloped using supercritical fluid extraction(SFE). The microcystins mcluded in the study are sparsely soluble in neat supercritical fluid CO$_2$ However, the microcystins were successfully extracted with a temary mixture(90% CO$_2$,9.0% methanol 1.0% water) at 40$^{\circ}$C and 250 atm. The SFE method developed in this study has several advantages over solid-phase extraction(SPE) sample preparation for the analysis of microcystins. Sample handling steps are minimized thus reducing possible losses of analytes and saving analysis time. No clean-up steps are employed in this SFE method. Althouhgh many methods have been described for microcystim RR and LR, the method using solid-phase extraction with ODS cartridges is the most commonly used. However, the adsorbing power of ODS caridges for microcystins is weak, so we have attempted to use a more polar CN cartridge, to increase the adsorbing power for microcystins. Lyophilized cells(100mg) were wxtracted with 5% (v/v) acetic acid. The extract was centrifuged and then the supernatant was applied to a CN cartridge. The cartridge which contained microcystins was rinsed with 5 ml of water and 5 ml of 0.5 M acetic acid. followed by 5 ml of 5% acetonitrile in water , and were determined by HPLC. Better recoveries and chromatogram were observed than with ODS cartridge.

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