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Development and Validation of Analytical Method for Decursin in Aerial Parts of Angelica gigas Nakai Extract (참당귀 지상부 추출물의 지표성분 decursin의 분석법 개발 및 검증)

  • Kim, Hee-Yeon;Lee, Ki-Yeon;Kim, Tae-Hee;Park, A-Reum;Noh, Hee-Sun;Kim, Si-Chang;Ahn, Mun-Seob
    • Journal of Food Hygiene and Safety
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    • v.34 no.1
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    • pp.52-57
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    • 2019
  • Method development and validation of decursin for the standardization of Angelica gigas Nakai as a functional ingredient and health food were accomplished. The quantitative determination method of decursin as a marker compound of aerial parts of Angelica gigas Nakai extract (AAGE) was optimized by HPLC analysis using a C18 column ($3{\times}150mm$, $3{\mu}m$) with 0.1% TFA in water and acetonitrile as the mobile phase at a flow rate of 0.5 mL/min and detection wavelength of 330 nm. The HPLC/PDA method was applied successfully to quantification of the marker compound in AAGE after validation of the method with linearity, accuracy, and precision. The method showed high linearity in the calibration curve at a coefficient of correlation ($R^2$) of 0.9994 and the limit of detection and limit of quantitation were $0.011{\mu}g/mL$ and $0.033{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 1.10% and 1.13%, respectively. Recovery of decursin at 0.5, 1, 5 and $10{\mu}g/mL$ were 92.38 ~ 104.11%. These results suggest that the developed HPLC method is very useful for the determination of marker compound in AAGE to develop a health functional material.

Study on Benzo(a)pyran Content and its Transfer Ratio in Extracts of Medicinal Herbs (한약재의 벤조피렌 함량 및 추출물에서의 이행률에 대한 연구)

  • Yoon, Hye-Min;Lee, Eun Ju;Lim, Kwang-Hee
    • Korean Chemical Engineering Research
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    • v.56 no.6
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    • pp.832-840
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    • 2018
  • In this study, both of the concentration of benzo(a)pyrene in 5 species (total 50 samples) of medicinal herbs and their transfer ratios in the preparation steps of water extract(decoction) and soft extract, were measured by HPLC/FLD. The calibration curve of benzo(a)pyrene shows excellent correlation over the concentration range of 3~40 ng/mL with the correlation coefficient ($R^2$) of 1.000. The detected benzo(a)pyrene concentrations from the medicinal herbs ranged from non-detection to $37.54{\mu}g/kg$, and their average was $6.73{\mu}g/kg$. Among the total samples, 15 samples (i.e., 30%) exceeded the limit of herbal medicine benzo(a)pyrene criteria (i.e., $5{\mu}g/kg$) according to the notification No. 2009-302 from Ministry of Food and Drug Safety. In particular, the concentration of benzo(a)pyrene in Coptidis Rhizome was turned out to be the highest of $37.54{\mu}g/kg$. The detected benzo(a)pyrene concentrations from water extract(decoction), soft extract and remnant after boiling, ranged from non-detection to $2.31{\mu}g/kg$, non-detection to $2.28{\mu}g/kg$, and 2.18 to $21.91{\mu}g/kg$, respectively. In preparation of water extract(decoction) and soft extract, transferred benzo(a)pyrene was not detected or, if transferred, the maximal transfer ratios of benzo(a)pyrene were shown to be 8.9% and 9.8%, respectively. Therefore, the content of benzo(a)pyrene in the samples of herbal medicine used in this study, were reduced by more than 90% in preparation steps of water extract (decoction) and soft extract.

Microbial Activity Analysis for the Selectively Sterilizing of Government-controlled Bulk Public Archives (대량 공공 기록물의 선별적 소독을 위한 미생물 활성도 분석 연구)

  • Kim, Dae Woon;Park, Ka Young;Kim, Ji Won;Kang, Dai Ill
    • Journal of Conservation Science
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    • v.34 no.6
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    • pp.443-458
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    • 2018
  • An archive is a collection of documents or records. Currently, most archived documents are made of paper. Paper is susceptible to biological damage and deterioration due to its material properties. To control the biological damage, treatment with chemical disinfectants and control of the storage environment are often used. In government-controlled bulk public archives, all documents are chemically sterilized before storage. However, an extremely large quantity of public records have been produced, and storage space and conservation management are gradually reaching their limits. In this study, 60 species of microbes were identified using a genetic method. We successfully applied the adenosine triphosphate (ATP) bioluminescence method to detect microbial contamination on paper documents. A calibration curve of the ATP bioluminescence as a function of the microbe quantity was obtained, and the microbial activity on non-sterilized paper archives from 1951 was analyzed using an ATP luminometer. It was found that the microbial activity was suppressed or reduced in climate-controlled storage environments at $22^{\circ}C$ and 55% relative humidity. We anticipate that these results will be used to establish selective sterilization systems for government-controlled bulk public archives.

A Study on the Migration of Heavy Metals from Polycarbonate Food Contact Materials Using an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) (식품용 폴리카보네이트 기구류 중 ICP-MS를 이용한 중금속 이행량 조사)

  • Park, Se-Jong;Park, So-Ra;Kim, MeeKyung;Choi, Jae Chun
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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    • v.24 no.3
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    • pp.107-112
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    • 2018
  • The purpose of this study was to investigate the migration levels of lead (Pb), cadmium (Cd) and arsenic (As) from polycarbonate food contact materials into food simulant at different temperatures ($70^{\circ}C$ and $100^{\circ}C$). The method was validated by linearity of calibration curves, limit of detection (LOD), limit of quantification (LOQ), recovery, precision and uncertainty. All of 200 samples, including bottles, cups, containers, ladles, spoons and tongs were purchased from domestic markets and analyzed by inductively coupled plasma mass spectrometry (ICP-MS). Mean concentrations of positive samples were higher at $100^{\circ}C$ than $70^{\circ}C$ as showing a dependency of migration temperature. The migration concentrations ranged from not-detected (ND) to $4.67{\mu}g/L$, ND to $0.49{\mu}g/L$L and ND to $2.91{\mu}g/L$ for Pb, Cd and As, respectively, which were far below the migration limits of Korea standards and specifications for food utensils, containers and packages.

Biological Accessibility to Algae Control through Measurement of Filtration Rate of Three Freshwater Bivalves (담수 이매패류 3종의 여과율 측정을 통한 조류 제어의 생물학적 접근 가능성)

  • Na, Young-Kwon;Kim, Dong-Kyun;Kim, Young-Shin;Park, Jung-Ho;Kwak, Ihn-Sil
    • Korean Journal of Ecology and Environment
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    • v.54 no.1
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    • pp.39-48
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    • 2021
  • In order to control algal bloom, which causes environmental problems such as eutrophication in freshwater ecological environments, many attempts have recently been made using biological approaches. Among them is filtration using bivalve. Algae control with filter-feeding bivalves is emerging as an eco-friendly method. In this study, bivalves collected at Baekje weir in Geum River in Korea from Jun to Sep 2020 were tested to find out the possibility of algae control using filter-feeding bivalves through laboratory experiments. The Unio douglasiae, Anodonta woodiana, and Anodonta arcaeformis collected from Baekje weir were put into a water tank (2 L) containing Clorella vulgaris, and as a result, the average filtration rate was 95.9% per animal after 24 hrs. Calculating this with the Chl-a concentration converted to a calibration curve, it was found that the average of 154.84 ㎍ L-1 of Chl-a was reduced. Based on this calculation, the possibility that one bivalve can eliminate Chl-a in one month is 0.0005%. It is expected that the effect is 20.14% when there are 40,000 animals. These results indirectly showed how effective bivalve's ability to control Chl-a in their habitat is. Although this study was limited to calculating the algae control ability of aquatic ecosystem based on the filtration rate of bivalve and the corresponding Chl-a reduction rate, it is thought that it will be used as basic data for integrated research from various factors and viewpoints (phytoplankton, aquatic plants, benthic organisms, and sediments) through additional research.

Determination of Sodium Alginate in Processed Food Products Distributed in Korea

  • Yang, Hyo-Jin;Seo, Eunbin;Yun, Choong-In;Kim, Young-Jun
    • Journal of Food Hygiene and Safety
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    • v.36 no.6
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    • pp.474-480
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    • 2021
  • Sodium alginate is the sodium salt of alginic acid, commonly used as a food additive for stabilizing, thickening, and emulsifying properties. A relatively simple and universal analysis method is used to study sodium alginate due to the complex pretreatment process and extended analysis time required during the quantitative method. As for the equipment, HPLC-UVD and Unison US-Phenyl column were used for analysis. For the pretreatment condition, a shaking apparatus was used for extraction at 150 rpm for 180 minutes at room temperature. The calibration curve made from the standard sodium alginate solution in 5 concentration ranges showed that the linearity (R2) is 0.9999 on average. LOD and LOQ showed 3.96 mg/kg and 12.0 mg/kg, respectively. Furthermore, the average intraday and inter-day accuracy (%) and precision (RSD%) were 98.47-103.74% and 1.69-3.08% for seaweed jelly noodle samples and 99.95-105.76% and 0.59-3.63% for sherbet samples, respectively. The relative uncertainty value was appropriate for the CODEX standard with 1.5-7.9%. To evaluate the applicability of the method developed in this study, the sodium alginate concentrations of 103 products were quantified. The result showed that the detection rate is highest from starch vermicelli and instant fried noodles to sugar processed products.

Analytical Method of Multi-Preservatives in Cosmetics using High Performance Liquid Chromatography (HPLC 를 이용한 화장품 중 살균보존제 다성분 동시분석법 연구)

  • Min-Jeong, Lee;Seong-Soo, Kim;Yun-Jeong, Lee;Byeong-Chul, Lee
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.48 no.4
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    • pp.321-330
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    • 2022
  • This study attempted to establish an optimal multi-compound simultaneous analysis method that can secure reliable results for 15 - preservatives, 2 - sun screens and 1 - antioxidants of cosmetics using HPLC-PDA. Since the potential of hydrogen (pH) in the mobile phase affects the acid dissociation constant (pKa) of the preservatives, and the peak retention time shift and area change were observed. The peak separation condition was established by adjusting the pH to 0.1% H3PO4 addition (mL) when preparing the mobile phase. As a results of method validation, the linearity correlation coefficient (R2) of above 0.999 were obtained, and accuracy 87.9 ~ 101.1%, 0.1 ~ 7.6% precision for two types of cosmetics (cream and shampoo). It was found that the limit of detection (LOD) was 0.1 ~ 0.2 mg/kg and the limit of quantitation (LOQ) was 2.0 ~ 4.0 mg/kg. In addition, it was possible to simultaneously separate p-anisic acid, a natural compound that was difficult to separate in HPLC due to the small difference from methylparaben, a synthetic preservatives. Through this study, it will be effectively used to secure quality control and safety for compound that need restrictions on use cosmetics.

Analysis Method of Surfactants for Identification of Residue Dishwashing Detergent (세척제 잔류량 확인을 위한 계면활성제 분석법 확립)

  • Park, Na-Youn;Lee, Sojeong;Kim, Jung Hoan;Kho, Younglim
    • Journal of the Korean Chemical Society
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    • v.65 no.6
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    • pp.433-440
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    • 2021
  • Surfactants are organic compounds that have both hydrophilic and non-polar parts in one molecule, classified as non-ion, anion, cation, and amphoteric surfactants according to the charge of hydrophilic parts in aqueous state. A trace amounts may remain when vegetables and fruits are washed using type1 detergent (Vegetable and fruit detergent), and there is a possibility of exposure to the human body through ingestion. This study developed the simultaneous analysis method for 5 surfactants with LC-MS/MS for analysis of detergent residues after washing vegetables and fruits with detergent. The mobile phase used distilled water and acetonitrile containing 50 mM ammonium formate and 0.1% formic acid and was analyzed using a gradient method using XBridge BEH C8 column. The accuracy of the established method was 83.9-112.1%, and the precision was less than 20%. The detection limit was 7.0 (SLS) to 29.0 (SLES-N3) ㎍/L, and the correlation coefficient (r2) of calibration line regression was greater than 0.99, it is considered suitable for the analysis of trace amounts of surfactant components remaining in vegetables and fruits.

The study on the measurement of formaldehyde in saliva and urine by GC-MS (가스크로마토그래프-질량분석기에 의한 타액 및 뇨 중 포름알데하이드 분석법 연구)

  • Shin, Ho-Sang;Ahn, Hye-Sil
    • Analytical Science and Technology
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    • v.19 no.2
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    • pp.149-154
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    • 2006
  • A gas chromatography-mass spectrometric method was developed for the determination of formaldehyde in urine and saliva. In a 20 mL glass tube, 0.2 mL of urine or saliva was taken. Further, 1.8 mL of 0.1 M HCl, 0.1 mL of 2,000 mg/L 2,4-dinitrophenyl hydrazine and $20{\mu}l$ of 500 mg/L acetone-$d_6$ as internal standard were added in the tube and sealed tightly with cap. The solution was shaken for 20 min at room temperature and extracted using 4 mL of toluene. The extract was concentrated and redissolved with $100{\mu}l$ of acetonitrile, and then measured by gas chromatography-mass spectrometer (selected ion monitoring). The detection limit was 2.0 ng/mL and 0.5 ng/mL in saliva and urine, respectively. The calibration curves showed good linearity with r = 0.997 and 0.998 for saliva and urine, respectively. The method was used to analyze formaldehyde in rat urine after oral exposure. The developed method may be use ful to the monitoring for formaldehyde exposure in human.

Rapid and simultaneous determination of metabolites of organic solvents in human urine by high-performance liquid chromatography using a monolithic column (Monolithic 칼럼을 이용한 뇨 중 유기용매 대사체의 신속한 HPLC 동시 분석)

  • Han, Sang Beom;Lee, Sang-Ju;Lee, Cheol-Woo;Yoon, Seo Hyun;Joung, Sun Kyung;Youm, Jeong-Rok
    • Analytical Science and Technology
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    • v.19 no.5
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    • pp.433-440
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    • 2006
  • A HPLC/UV method was developed and validated for the rapid and simultaneous determination of urinary metabolites of organic solvents, mandelic acid, hippuric acid, phenylglyoxylic acid, ortho-, meta- and para-methylhippuric acid, using a monolithic column. The mobile phase was composed of tetrabutylammonium bromide as ion-pairing reagent with a flow rate of 2.4 mL/min. The total run time was less than 2.5 min for all six analytes. Good linearities were obtained for all the metabolites with correlation coefficients above 0.9993. Intra-day precision, accuracy and inter-day precision was 0.01~7.32%, 83.9~116.3% and 0.01~7.16%, respectively. The method was validated and confirmed by quantification of the quality assurance samples of Industrial Safety and Health Research Institute, Korea Occupational Safety and Health Agency.