• Title/Summary/Keyword: Gas Chromatography-Mass Spectrometry

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Analysis of an ancient textiles from the Xianbei period tombs of the Shiveet Khairkhan site, Mongolia (몽골 시베트 하이르한 유적 선비 시기(1~3세기) 고분 출토 직물의 섬유와 염료 분석)

  • YUN Eunyoung;YU Jia;PARK Serin;AN Boyeon
    • Korean Journal of Heritage: History & Science
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    • v.55 no.4
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    • pp.166-177
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    • 2022
  • The Shiveet Khairkhan is located on Tsengel Som in the middle of Bayan-ulgi Aimag in the Altai region. Various remains have been identified, and it has been found to be an important area of the Eurasian steppe. In this study, the characteristics of textile fibers and dyes excavated from the tombs of the 1st~3rd century Xianbei period in the sites of Shiveet Khairkhan, Mongolia were investigated. As a result of analysis using optical microscopic observation and attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) for fiber identification, green and yellow fabrics were identified as silk fabrics. To investigate the properties of the dye, the surface reflectance of the dyed fabric was measured using an fiber optic reflectance spectrophotometer for non-destructive analysis. The green fabric appeared similar to the reflection spectrum of indigo dye. In addition, as a result of component analysis using gas chromatography-mass spectrometry, isatin and indigotine were detected. Isatin and indigotine are characteristic components of indigo dye, and it was found that the green fabric of the tombs of the Xianbei period was dyed using indigo dye. It was difficult to identify the type of dye in the yellow fabric as a result of reflectance spectrum and gas chromatography analysis. Indigo plants are a dye used for blue dyeing from thousands of years ago, and many species are distributed around the world. It was confirmed that the fabric was relatively well preserved and indigo dye was used for the green Jikryeongui (garment with a straight collar) in the ancient tomb of the Xianbei period about 1,800 years ago, even though it was buried for a long time. Scientific investigation of textile cultural heritage is an essential process for conservation treatment, restoration, exhibition, and the creation of a conservation environment. It is expected that related research will be activated in the future and will be helpful in interpreting the living culture at the time, preserving textiles, and a conservation environment.

Monitoring and Risk Assessment of Pesticide Residues Farmers' Market Produce in Northern Gyeonggi-do (경기 북부 내 직거래 농산물의 잔류농약 실태조사 및 위해성 평가)

  • Lim, Jeong-Hwa;Park, Po-Hyun;Lim, Bu-Geon;Ryu, Kyong-Shin;Kang, Min-Seong;Song, Seo-Hyeon;Kang, Nam-Hee;Yoo, Na-Young;Kim, Jeong-Eun;Kang, Choong-Won;Kim, Youn-Ho;Seo, Jeong-Hwa;Choi, Ok-Kyung;Yoon, Mi-Hye
    • Journal of Food Hygiene and Safety
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    • v.35 no.3
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    • pp.243-251
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    • 2020
  • In this study, we investigated pesticide residues in 207 agricultural products distributed by direct trade in the northern area of Gyeonggi Province. A total of 94 general agricultural products and 113 eco-friendly agricultural products collected from local grocers and cooperative stores were analyzed by multiresidue method for 263 pesticides using GC (gas chromatography)/ECD (electron capture detector), GC/NPD (nitrogen phosphorus detector), GC-MS/MS (tandem mass spectrometry), LC (liquid chromatography)/PDA (photodiode array detector), LC/FLD (fluorescence detector), LC-MS/MS. All samples showing pesticide residues were general agricultural products collected from local food stores. The pesticide residue levels of 14 samples (6.8%) were below the maximum residue limits (MRLs) and one of them (0.5%) exceeded the MRLs. Sixteen pesticides were detected from samples of the following produce items: spinach, young cabbage, perilla leaves, mallow, cucumber, chives and water dropwort. The safety of the detected pesticides was assessed by monitoring the daily intake estimate (EDI) and the daily intake allowance (ADI) based on the amount of pesticides detected. The ADI percentage range (the ratio of EDI to ADI) was 0.0134-61.6259% and there was no health risk connected with consuming agricultural products in which pesticide residues were detected.

A Study of Current Status on Pesticide Residues in Commercial Dried Agricultural Products (서울시 유통 건조농산물 중의 농약잔류 실태 연구)

  • Kim, Bog-Soon;Park, Seoung-Gyu;Kim, Mi-Sun;Cho, Tae-Hee;Han, Chang-Ho;Jo, Han-Bin;Choi, Byung-Hyun;Kim, Sung-Dan
    • Korean Journal of Food Science and Technology
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    • v.39 no.2
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    • pp.114-121
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    • 2007
  • The purpose of this study was to investigate 253 kinds of pesticide residues in 58 commercial dried agricultural products in Seoul. The determinations of the pesticide residues were performed using multiresidue methods and were carried out by a gas chromatography-nitrogen phosphorus detector (GC-NPD), an electron capture detector ($GC-{\mu}ECD$), a mass spectrometry detector (GC-MSD) and high performance liquid chromatography-ultraviolet detector (HPLC-UV), and a fluorescence detector (HPLC-FLD). The pesticide residue detection rate in the commercial dried agricultural products was 24.1% (14 of 58 samples). Twelve pesticide residues without maximum residue limits (MRLs) were detected. In the vegetable groups, the frequency of pesticide residues was found to be in the increasing order of dried fruiting vegetables > dried leafy vegetables > dried stalk and stem vegetables. The pesticides used on dried red pepper in the dried fruiting vegetables were varied (7 kinds) and numerous (4 of 8 samples). The pesticide types detected in the commercial dried agricultural products were in the order of pyrethroid > organochloride > organophosphorus and insecticide > fungicide > herbicide ${\cdot}$ nematicide. The primary pyrethroid pesticide detected was cypermethrin. According to the producing areas of products, large numbers of pesticide residues were found in the order of Korea, China, North Korea, USA, and Vietnam.

Study on the Analytical Method and Monitoring of the Oxidized Polyethylene Wax in Foods (식품 중 oxidized polyethylene wax 분석법 연구 및 함유량 실태 조사)

  • Choi, Seung-Hyun;Kim, Jae-Min;Choi, Sun-il;Jung, Tae-Dong;Cho, Bong-Yeon;Lee, Jin-Ha;Lee, Gunyoung;Lim, Ho Soo;Yun, Sang Soon;Lee, Ok-Hwan
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.284-289
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    • 2017
  • Oxidized polyethylene wax (OPEW) is, one of the food additives, used as a coating agent in citrus fruits and nuts. OPEW is authorized to quantum satis in EU, USA, and is acceptable less than 250 mg/kg in Australia and New Zealand. But OPEW is unauthorized as a food additive in Korea. This study was to establish the analytical method of OPEW and demonstrate the effective application of various food samples. We first conducted to compare the various analytical method including acid value (AV), high temperature gel permeation chromatography (HT-GPC), matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF/MS), gas chromatography flame ionization detector (GC-FID) and fourier transform infrared spectroscopy (FT-IR). This result indicated that FT-IR spectrum of OPEW treated food sample displayed absorption bands for carbonyl group (C=O, $1714cm^{-1}$), ester group (C-O, $1463cm^{-1}$), aliphatic group (C-H, $2916cm^{-1}$). Furthermore, IR spectrum of OPEW treated food sample showed similar tendency with IR spectrum of OPEW standard. Therefore, it is confirmed that analytical method using FT-IR can be detected on analysis of OPEW in food. As a result of monitoring of 111 samples using established analytical method, OPEW was not detected in the food samples.

Detection of Hydrocarbons Induced by Electron Beam Irradiation of Almond (Prunus amygosalus L.) and Peanut (Arachis hypogaea) (전자선 조사한 아몬드(Prunus amygosalus L.)와 땅콩(Arachis hypogaea)에서 유래한 지방분해산물 분석)

  • Jeong, In Seon;Kim, Jae Sung;Hwang, In Min;Choi, Sung Hwa;Choi, Ji Yeon;Nho, Eun Yeong;Khan, Naeem;Kim, Byung Sook;Kim, Kyong Su
    • Korean Journal of Food Science and Technology
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    • v.45 no.1
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    • pp.20-24
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    • 2013
  • Food irradiation has recently become one of the most successful techniques to preserve food with increased shelf life. This study aims to analyze hydrocarbons in almonds (Prunus amygosalus L.) and peanuts (Arachis hypogaea) induced by electron beam irradiation. The samples were irradiated at 0, 1, 3, 5 and 10 kGy by e-beam and using florisil column chromatography fat, and content was extracted. The induced hydrocarbons were identified using gas chromatography-mass spectrometry (GC/MS). The major hydrocarbons in both irradiated samples were 1,7-hexadecadiene ($C_{16:2}$) and 8-heptadecene ($C_{17:1}$) from oleic acid, 1,7,10-hexadecatriene ($C_{16:3}$) and 6,9-heptadecadiene ($C_{17:2}$) from linoleic acid and 1-tetradecene ($C_{14:1}$) and pentadecane ($C_{15:0}$) from palmitic acid. Concentrations of the hydrocarbons produced by e-beam were found to be depended upon the composition of fatty acid in both almonds and peanuts. The $C_{n-2}$ compound was found to be higher than $C_{n-1}$ compound in oleic acid and palmitic acid, while in case of linoleic acid, $C_{n-1}$compound was higher than $C_{n-2}$ compound. The radiation induced hydrocarbons were detected only in irradiated samples, with 1 kGy or above, and not in the non-irradiated ones. The production of 1,7-hexadecadiene ($C_{16:2}$), 8-heptadecene ($C_{17:1}$), 1,7,10-hexadecatriene ($C_{16:3}$) and 6,9-heptadecadiene ($C_{17:2}$), in high concentration gave enough information to suggest that these may be the possible marker compounds of electron beam irradiation in almonds and peanuts.

Establishment of an Analytical Method for Prometryn Residues in Clam Using GC-MS (GC-MS를 이용한 바지락 중 prometryn 잔류분석법 확립)

  • Chae, Young-Sik;Cho, Yoon-Jae;Jang, Kyung-Joo;Kim, Jae-Young;Lee, Sang-Mok;Chang, Moon-Ik
    • Korean Journal of Food Science and Technology
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    • v.45 no.5
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    • pp.531-536
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    • 2013
  • We developed a simple, sensitive, and specific analytical method for prometryn using gas chromatography-mass spectrometry (GC-MS). Prometryn is a selective herbicide used for the control of annual grasses and broadleaf weeds in cotton and celery crops. On the basis of high specificity, sensitivity, and reproducibility, combined with simple analytical operation, we propose that our newly developed method is suitable for use as a Ministry of Food and Drug Safety (MFDS, Korea) official method in the routine analysis of individual pesticide residues. Further, the method is applicable in clams. The separation condition for GC-MS was optimized by using a DB-5MS capillary column ($30m{\times}0.25mm$, 0.25 ${\mu}m$) with helium as the carrier gas, at a flow rate of 0.9 mL/min. We achieved high linearity over the concentration range 0.02-0.5 mg/L (correlation coefficient, $r^2$ >0.998). Our method is specific and sensitive, and has a quantitation limit of 0.04 mg/kg. The average recovery in clams ranged from 84.0% to 98.0%. The reproducibility of measurements expressed as the coefficient of variation (CV%) ranged from 3.0% to 7.1%. Our analytical procedure showed high accuracy and acceptable sensitivity regarding the analytical requirements for prometryn in fishery products. Finally, we successfully applied our method to the determination of residue levels in fishery products, and showed that none of the analyzed samples contained detectable amounts of residues.

Case Study on Determination of the Level of New RoHS II Substances in Domestic Electronic and Electrical Equipments (국내 전기전자 제품에 함유된 신규 RoHS II 물질 검출 사례 연구)

  • Song, Moon-Hwan;Son, Seung-Hwan;Cho, Young-Dal;Choe, Eun-Kyung
    • Clean Technology
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    • v.17 no.2
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    • pp.124-133
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    • 2011
  • In addition to six substances regulated in EU RoHS including lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyls (PBB) and polybrominated diphenyl ethers (PBDE), priority substances are identified in new RoHS II as hexabromocyclododecane (HBCDD), dibutyl phthalate (DBP), butyl benzyl phthalate (BBP) and diethylhexyl phthalate (DEHP). In this study, 20 plastic samples were collected from 12 domestic electrotechnical companies and levels of four restricted substances were determined by gas chromatography-mass spectrometry, Among 20 parts that compose washer, refrigerator or microwave oven, HBCDD was detected in three samples of NBR material with the amount of 42~381 mg/kg while DBP and BBP was not detected in any samples collected respectively, implying that these substance may not be used widely in plastic materials for EEE. However, DEHP was detected in all samples of NBR, PP, PBT, EPDM and PVC materials with the amount of 42 up to 59,400 mg/kg that exceeds the limit value of 0.1 wt% (1,000 mg/kg). Presence of a restricted substance in polymer material makes a great negative influence on a number of final product. To cope with coming RoHS II as well as REACH, action not to use DEHP in plastic material or the relevant notification in case of REACH seems to be needed. Screening test of Arsenic compounds such as diarsenic pentaoxide, diarsenic trioxide, lead hydrogen arsenate, triethyl arsenate that are included in REACH SVHC was done by ICP measurement Arsenium was detected in four samples made of NBR and PBT materials in the level of 15~700 mg/kg. By considering the screening method used in this study, the amount of arsenium compounds in the thermistor made of PBT material has a high chance of exceeding the regulated limit value.

A Survey on Endocrine Disrupting Chemicals in Animal Wastes Treated with Methane Fermentation (메탄발효 처리된 가축분뇨내의 내분비계 장애물질에 대한 조사 연구)

  • Ko, H.J.;Kim, K.Y.;Kim, H.T.;Umeda, M.
    • Korean Journal of Environmental Agriculture
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    • v.26 no.1
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    • pp.62-68
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    • 2007
  • Concerns about endocrine disrupting chemicals emitted from humans and animals have been increased because these compounds are detected at very low levels in environment and adversely affect on indigenous fauna. To date, there is little information regarding the concentration of these compounds in animal wastes. In this study, the female hormones, $17\beta-estradiol$ (E2), estrone (E1) and estriol, were measured to provide baseline data in animal wastes. Samples were collected from animal waste storage, methane digester and sludge separated wastewater and analyzed by gas chromatography-mass spectrometry. To measure the mass ratios of estrogen to macronutrients, nitrogen and phosphorous were also determined. Sample collected from animal waste storage had the highest estrogen concentration (98.7 ${\mu}g/L$), while sludge separated wastewater had the lowest concentration (3.4 ${\mu}g/L$). The mean concentrations of E2 and E1 in waste storage sample were (6.8 ${\mu}g/L$) and (68.7 ${\mu}g/L$), respectively. In sludge separated wastewater, the mean concentration of both E2 and E1 were reduced to (2.6 ${\mu}g/L$) and (1.9 ${\mu}g/L$), respectively. However, estriol was not detected in any of the samples collected. Mean ratios of E2 and E1 to macronutrients were significantly different between the methane wastewater and sludge separated wastewater owing to elimination of solid particles.

The Monitoring on Plasticizers and Heavy Metals in Teabags (침출용 티백 포장재의 안전성에 관한 연구)

  • Eom, Mi-Ok;Kwak, In-Shin;Kang, Kil-Jin;Jeon, Dae-Hoon;Kim, Hyung-Il;Sung, Jun-Hyun;Choi, Hee-Jung;Lee, Young-Ja
    • Journal of Food Hygiene and Safety
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    • v.21 no.4
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    • pp.231-237
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    • 2006
  • Nowadays the teabag is worldwide used for various products including green tea, tea, coffee, etc. since it is convenient for use. In case of outer packaging printed, however, there is a possibility that the plasticizers which is used for improvement in adhesiveness of printing ink may shift to inner tea bag. In this study, in order to monitor residual levels of plasticizers in teabags, we have established the simultaneous analysis method of 9 phthalates and 7 adipates plasticizers using gas chromatography (GC). These compounds were also confirmed using gas chromatography-mass spectrometry (GC-MSD). The recoveries of plasticizers analyzed by GC ranged from 82.7% to 104.6% with coefficient of variation of $0.6\sim2.7%$ and the correlation coefficients of each plasticizer was $0.9991\sim0.9999$. Therefore this simultaneous analysis method was showed excellent reproducibility and linearity. And limit of detection (LOD) and limit of quantitation (LOQ) on individual plasticizer were $0.1\sim3.5\;ppm\;and\;0.3\sim11.5\;ppm$ respectively. When 143 commercial products of teabag were monitored, no plasticizers analysed were detected in filter of teabag products. The migration into $95^{\circ}C$ water as food was also examined and the 16 plasticizers are not detected. In addition we carried out analysis of heavy metals, lead (Pb), cadmium (Cd), arsenic (As) and aluminum (Al) in teabag filters using ICP/AES. $Trace\sim23{\mu}g$ Pb per teabag and $0.6\sim1718{\mu}g$ Al per teabag were detected in materials of samples and Cd and As are detected less than LOQ (0.05 ppm). The migration levels of Pb and Al from teabag filter to $95^{\circ}C$ water were upto $11.5{\mu}g\;and\;20.8{\mu}g$ per teabag, respectively and Cd and As were not detected in exudate water of all samples. Collectively, these results suggest that there is no safety concern from using teabag filter.

An Improved Analytical Method for the Determination of Qualitative and Quantitative Characteristics of Di- and Trisaccharides in Honey using GC and GC/MS (GC 및 GC/MS에 의한 벌꿀 중의 이·삼당류 정성 및 정량 특성과 개선된 동시분석방법의 확립)

  • Kim, Jong-Bae;Jang, Eun-Suk;Kim, In-Suk;Lee, Hee-Jin;Lee, Hye-Jeong;Seo, Hyun-Sun;Park, Nam-Pyo
    • Korean Journal of Food Science and Technology
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    • v.47 no.1
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    • pp.27-36
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    • 2015
  • The improved analytical method with gas chromatography (GC) and GC-mass spectrometry was established to identify and quantify disaccharides and trisacchrides in honey. In this method, the analysis of trimethylsilyl (TMS), TMS-oxime and TMS-methoxime sugars takes into account the determination of a single peak of complete separation on the chromatogram. The number of possible peaks for the qualitative and quantitative determination of TMS, TMS-oxime, and TMS-methoxime sugars was 17, 22, and 25, respectively. This new analytical method allowed for the determination of diand trisaccharides in honey by TMS-oxime and TMS-methoxime derivatives. This study suggested that the improved method is more suitable and precise than the other analytical methods for the simultaneous determination of sugars in honey.