• Title/Summary/Keyword: GC-FID/MS

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Compositions of fatty acids and structural identification in human breast milk (모유 중 지방산 조성 및 구조 분석)

  • Ji-Woo, Yoo;Young-Soo, Keum;Nam Mi, Kang
    • Analytical Science and Technology
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    • v.35 no.6
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    • pp.229-236
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    • 2022
  • Lipidomic analyses of transient breast milk are far more limited than those of other dairy products. As a preliminary analysis of breast milk lipidomes, analytical methods for polar and nonpolar lipids from transient breast milk were developed, and detailed fatty acid profiles were determined in this study. The newly developed methods include solvent fractionation of phospholipids and acyl glycerol, one-pot derivatization to FAMEs and pyridylcarbinol esters, and instrumental analysis, including GC-FID and GC-MS. The results indicate that breast milk contains 16 major common fatty acids with 8-22 carbons. Additionally, 29 minor fatty acids were identified, including odd-numbered fatty acids and branched analogues with 11-23 carbons. Their detailed concentrations in different fractions were measured using the internal standard method. In addition to ordinary fatty acids, breast milk contains several branched fatty acids, including iso/anteiso acids with 15-18 carbons. Structural studies have been performed on selected minor fatty acids via chemical synthesis.

A Study on Migration of Ethylenediamine and Hexamethylenediamine from Polyamide Utensils (Polyamide 조리기구로부터 Ethylenediamine 및 Hexamethylenediamine의 이행에 관한 연구)

  • Eom, Mi-Ok;Kwak, In-Shin;Yoon, Hae-Jung;Jeon, Dae-Hoon;Choi, Hyun-Chul;Kim, Hyung-Il;Sung, Jun-Hyun;Park, Na-Young;Kim, So-Hee;Lee, Young-Ja
    • Journal of Food Hygiene and Safety
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    • v.25 no.1
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    • pp.36-42
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    • 2010
  • The method for the determination of ethylenediamine (EDA) and hexamethylenediamine (HMDA) in food simulants was developed, and migration amounts of these compounds was monitored for 124 polyamide (PA) utensils. The diurethane derivatives of EDA and HMDA, which produced by reaction with ethyl chloroformate, were analyzed by using gas chromatograph (GC)/flame ionization detector (FID) and GC/mass spectrometer (MS). The developed method was validated with $0.3\;{\mu}g/mL$ of limit of detection (LOD) for EDA and $0.1\;{\mu}g/mL$ of LOD for HMDA, > 0.999 of linearity($r^2$) and > 88% of recovery. The EDA was detected 1.31 and $02.06\;{\mu}g/mL$ for 2 samples in water. The HMDA was detected $0.29\;-\;0.93\;{\mu}g/mL$ for 3 samples in 20% ethanol and $0.26\;-\;0.44\;{\mu}g/mL$ for 10 samples in n-heptane. These migration levels were below the specific migration limits (SML) of $12\;{\mu}g/mL$ and $2.4\;{\mu}g/mL$ for EDA and HMDA established in EU.

Development and Validation of Analytical Method for Determination of Biphenyl Analysis in Foods (식품 중 비페닐 분석법 개발 및 유효성 검증)

  • Kim, Jung-Bok;Kim, Myung-Chul;Song, Sung-Woan;Shin, Jae-Wook
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.4
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    • pp.459-464
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    • 2017
  • Biphenyl is used as an intermediate in the production of crop protection products, a solvent in pharmaceutical production, and as a component in the preservation of citrus fruits in many countries. Biphenyl is not authorized for use and also does not have standards or specifications as a food additive in Korea. National and imported food products are likely to contain biphenyl. Therefore, control and management of these products is required. In this study, a simple analytical method was developed and validated using HPLC to determine biphenyl in food. These methods are validated by assessing certain performance parameters: linearity, accuracy, precision, recovery, limit of detection (LOD), and limit of quantitation (LOQ). The calibration curve was obtained from 1.0 to $100.0{\mu}g/mL$ with satisfactory relative standard deviations (RSD) of 0.999 in the representative sample (orange). In the measurement of quality control (QC) samples, accuracy was in the range of 95.8~104.0% within normal values. The inter-day and inter-day precision values were less than 2.4% RSD in the measurement of QC samples. Recoveries of biphenyl from spiked orange samples ranged from 92.7 to 99.4% with RSD between 0.7 and 1.7% at levels of 10, 50, and $100{\mu}g/mL$. The LOD and LOQ were determined to be 0.04 and $0.13{\mu}g/mL$, respectively. These results show that the developed method is appropriate for biphenyl identification and can be used to examine the safety of citrus fruits and surface treatments containing biphenyl residues.

Studies on the Effect of Low Winter Temperatures and Harvest Times on the Volatile Aroma Compounds in Green Teas (동절기 저온현상과 채엽시기에 따른 녹차의 향기성분에 대한 연구)

  • Ryu, Kyung-Heon;Lee, Hye-Jin;Park, Seung-Kook
    • Korean Journal of Food Science and Technology
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    • v.44 no.4
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    • pp.383-389
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    • 2012
  • Green tea leaves grown in Jeju island were harvested at different times in 2010 and 2011. Green teas harvested in 2010 experienced higher effective accumulative temperature than green teas harvested in 2011. The free and bound volatile compounds in green tea were analyzed using headspace-solid phase microextraction gas chromatography (GC) and GC-mass spectrometry. All green teas contained the 6 major volatile compounds ${\alpha}$-methylbutanal, pentanal, (E)-2-hexen-1-ol, ${\beta}$-linalool, geraniol and ${\alpha}$-farnesene. After enzyme treatment, (Z)-3-hexen-1-ol, benzaldehyde, (Z)-3-hexenyl acetate, ${\beta}$-linalool and geraniol were increased in all green teas. (Z)-3-hexen-1-ol increased significantly in green tea harvested in 2010, and benzaldehyde increased widely in green tea harvested in 2011. However, the total volatile compounds in green teas harvested in 2011 were remarkably decreased in comparison to harvested in 2010. It was confirmed that free and bound volatile compounds in green tea are affected by low winter temperatures.

Proximate, Free Sugar, Fatty acids Composition and Anthocyanins of Saekso 2 Corn Kernels (옥수수 색소 2호 품종의 일반성분, 유리당, 지방산 및 안토시아닌 색소의 함량)

  • Lee, Ki Yeon;Kim, Tae hee;Lim, Sang Hyun;Park, Jong yeol;Kim, Kyung Hee;Ahn, Mun Seob;Kim, Hee Yeon
    • Journal of Food Hygiene and Safety
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    • v.31 no.5
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    • pp.335-341
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    • 2016
  • This study was performed to provide basic data of Saekso 2 corn kernels. Proximate composition, free sugars, fatty acids and anthocyanin content of Saekso 2 corn kernels were analyzed. Proximate composition of dried Saekso 2 corn kernels were represented 8.84% moisture, 1.44% crude ash, 5.46% crude lipid, 10.31% crude protein. Free sugars composition by HPLC/ELSD showed that sucrose (1.00%), glucose (0.63%), maltose (0.52%), fructose (0.44%) were present. The composition of fatty acids in Saekso 2 corn kernels was analyzed by GC/FID. 11 species of fatty acids were analyzed in Saekso 2 corn kernels. The ratio of saturated fatty acids and unsaturated fatty acids 16.09 : 83.91. Content of linoleic acid was the highest in fatty acids. The total anthocyanin content in Saekso 2 corn kernels was 0.24% by UV/Vis. Anthocyanin components separated and quantified using HPLC/MS/MS. Cyanidin 3-O-glucoside chloride (C-3-G), pelargonidin 3-O-glucoside chloride (Pg-3-G) and peonidin 3-O-glucoside chloride (Pn-3-G) of anthocyanin were analyzed in Saekso 2 corn kernels.

A comparative analysis of volatile organic compound levels in field samples between different gas chromatographic approaches (분석기법의 차이에 따른 현장시료의 VOC 분석결과 비교연구: 분석오차의 발생 양상과 원인)

  • Ahn, Ji-Won;Pandey, Sudhir Kumar;Kim, Ki-Hyun
    • Analytical Science and Technology
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    • v.23 no.5
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    • pp.465-476
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    • 2010
  • In this study, a number of volatile organic compounds (VOCs) including benzene, toluene, p-xylene, styrene, and methyl ethyl ketone were analyzed from samples collected in ambient air and under the field conditions. These samples were analyzed independently by two different set-ups for VOC analyses, i.e., between [1] gas chromatography/flame ionization detector with tube sampling - (F-T system) and [2] gas chromatography/mass spectrometer with bag sampling (M-B system). The analytical results derived by both systems showed fairly similar patterns in relative sense but with moderately large differences in absolute sense. The results of M-B system were high relative to F-T system with the F-T/M-B ratio below 1. If the relative biases of the two measurement techniques are derived in terms of percent difference (PD) in concentration values, the results were generally above 35% on average. A student t-test was applied to investigate the statistical significance of those differences between the systems. The results of both analytical systems were different at 95% confidence level for toluene, p-xylene, styrene, and methyl ethyl ketone (P < 0.043). However, F-T and M-B systems showed strong correlations for toluene and p-xylene. The observed bias is explained in large part by such factors as the differences in standard phases used for each system and the chemical loss inside the bag sampler.

Application of the Latest European Standard(EN 15522-2) for Marine Oil Spill Analysis: A Study on its Effectiveness in Analyzing Samples from Korean Incidents (해양 기름유출사고 분석을 위한 최신 유럽표준(EN 15522-2) 적용: 한국 사고 샘플 분석의 효율성에 관한 연구)

  • Youjeong Park;Duwon Lee;Heejin Lee
    • Journal of the Korean Society of Marine Environment & Safety
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    • v.30 no.1
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    • pp.58-64
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    • 2024
  • Approximately 250 marine oil spill accidents have occurred in Korea, with profound impact on local communities and the environment. The restoration process necessitates significant resources and costs to return affected areas to their pre-accident state. In accordance with the polluter pays principle, compensation is demanded from polluter, as stipulated in both international conventions and national laws. Consequently, investigations are conducted to determine civil and criminal liability. As the importance of investigation actors in oil spill accidents increases, standards such as CEN 15522-2 and ASTM D 3248 are employed to determine the similarity between the spilled oil and the oil of the suspected ship. Among these standards, CEN 15522-2, the most actively used European standard, underwent its third revision and is now known as EN 15522-2, as of 2023. This study used EN 15522-2 to analyze samples from marine oil spill accidents that occurred in Korea. The results indicated that, considering the characteristics of domestic spills where light fuel oil spills account for more than 40%, the application of EN 15522-2, which includes low-boiling point substances such as Adamantanes, was confirmed to be highly effective.

A Study on Migration of Monomers from Kitchen Utensils Including PA, PU, ABS, and Acrylic Resin Plastics (폴리아마이드제 등 조리기구 중 모노머의 이행에 관한 연구)

  • Choi, Jae-Chon;Park, Se-Jong;Park, Geon-Woo;Min, Hye-Kyoung;Yang, Ji-Young;Kim, Meehye
    • Journal of Food Hygiene and Safety
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    • v.30 no.1
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    • pp.81-86
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    • 2015
  • The purpose of our paper was to investigate the migration level of 4,4'-MDA(4,4'-methylenedianiline), 2,4-TDA(2,4-toluenediamine), aniline, acrylonitrile and methylmeth acrylate from plastic cookwares into food simulants and to evaluate the safety of each monomers. The test articles for monomers were PA (polyamide) items for 4,4'-MDA, 2,4-TDA and aniline, PU (polyurethane) items for 4,4'-MDA, ABS (acrylonitrile-butadiene- styrene) items for acrylonitrile, and acrylic resin items for methylmethacrylate. All the article samples of 321 intended for contact with foods were purchased in domestic market. 4,4'-MDA, 2,4-TDA and aniline were analyzed by LC-MS/MS (liquid chromatography -tandem mass spectrometer), acrylonitrile by GC-NPD (gas chromatography-nitrogen phos phorus detector) and methyl methacrylate by GC-FID (gas chromatography-flame ionization detector). The migration level of monomers were within the migration limits of Ministry of Food and Drug Safety (MFDS). As a result of safety evaluation, our results showed that the estimated daily intake (EDI, mg/kg bw/day)s were $2.39{\times}10^{-9}$ and $1.20{\times}10^{-9}$ for 4,4'-MDA and 2,4-TDA of PA, $4.32{\times}10^{-9}$ for acrylonitrile of ABS and $2.27{\times}10^{-7}$ for methylmethacrylate of acrylic resin. Reference Dose (RfD, mg/kg bw/day) of acrylonitrile and tolerable daily intake (TDI, mg/kg bw/day) of methacrylate were established respectively as 0.001 by EPA (US Environmental Protection Agency) and as 1.2 by WHO (World Health Organization). When comparing with RfD and TDI, the EDIs of acrylonitrile and methylmethacrylate accounted for $4.32{\times}10^{-4}%$ and $1.89{\times}10^{-5}%$ respectively.

Comparison of Chemical Constituents in Mung bean (Vigna radiata L.) Flour between Cultivation Regions and Seeding Dates

  • An, Yeon Ju;Kim, Mi Jung;Han, Sang Ik;Chi, Hee-Youn;Kwon, Chang;Kim, So Yeon;Yang, Yu Jin;Kim, Yun Ju;Moon, Hee Sung;Kim, Seung-Hyun;Chung, Ill-Min
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.65 no.4
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    • pp.457-467
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    • 2020
  • Legumes are one of the largest families of crop plants and are widely consumed and produced for their nutritional and commercial benefits. Mung bean (Vigna radiata L.) is a legume crop that contains various functional compounds ; moreover, it has strong antioxidant properties and is becoming an increasingly important food crop. However, most previous studies on mung beans have focused on their primary metabolites. In this study, we investigated the composition and contents of phenolic compounds, fatty acids, soyasapogenol and tocopherol in mung beans cultivated in different regions and cultivated at different seeding dates. Material analysis was conducted using the following methods: LC-MS/MS, GC-FID and HPLC-ELSD. In total, 57 different samples were analyzed. Thirteen phenolic compounds were detected in mung beans. Of these, vitexin and isovitexin were the most abundant compounds, accounting for approximately 99% of phenolic compounds. The difference in phenol compounds according to the seeding dates of mung bean was not statistically significant. The total fatty acid content in beans was the highest in Pyeongchang. Significant differences in total fatty acid content were found according to the cultivation regions. Crops grown in Sohyeon and Dahyeon showed the highest soyasapogenol B content in the Suwon region, and these were the lowest in Jeonju. The total tocopherol content of beans cultivated in Dahyeon and Sohyeon was the lowest and highest in Pyeongchang. Soyasapogenol B and total tocopherol content were not significantly different according to seeding dates. This study was conducted to obtain basic data for the cultivation of mung beans with a high content of various functional materials in terms of regional specialization and optimal seeding time.

Analysis of Chemical Components for Aerial and Underground Parts of Wild Ginseng and Evaluation of Skin Anti-aging Efficacy (야생 산삼 지상부 및 지하부의 화학성분 분석과 피부 항노화 효능 평가)

  • Seok-Seon Roh;Gwang Jin Lee;Byunghyun Kim;Bo Kyoung Hwang;Hyojin Kim;Yun Hee Chang;Jae-kun Yoou;Young-Sung Ju
    • The Korea Journal of Herbology
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    • v.38 no.5
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    • pp.85-95
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    • 2023
  • Objectives : This study was intended to reveal the chemical profiles of aerial(leaf, stem) and underground(rhizome, radix) parts of wild ginseng, and to investigate their anti-aging effects on human skin cells. Methods : Wild ginseng, estimated for over 20 years, was divided into the aerial and underground parts. Total phenolic contents of each extracts were measured using a Folin-ciocalteu method. The contents of 18 amino acids, 8 minerals and 27 ginsenosides were determined by GC-FID, ICP-MS and LC-MS, respectively. The anti-aging effects, including the radical scavenging activity, the activation of mitochondrial function on human fibroblasts, and the proliferation activity on human keratinocyte progenitor cells, for the whole plant and underground part of wild ginseng were evaluated. Results : The total phenolic acids, amino acids, and minerals in the aerial part were more than twice as high as in the underground part. Compared to the cultivated ginseng root, there were various types of ginsenosides in both parts of wild ginseng, and the total amount was more than twice as high. In particular, the aerial part significantly contained ginsenoside F1, F2, C-Mc1, and C-O, and the distinctive patterns that distinguish each parts of wild ginseng from the cultivated ginseng root were derived. The whole plant and underground part of wild ginseng exhibited significant antioxidant effect(14.3-45.6%), activation of mitochondrial membrane potential(105.5-120.1%), and cell proliferation(112.1-125.4%). Conclusions : The entire plant and underground part of wild ginseng are high value-added plants and have beneficial effects on skin anti-aging properties through its abundant metabolites.