• Title/Summary/Keyword: Mass spectrometry

Search Result 3,346, Processing Time 0.037 seconds

Development of simultaneous analytical method for investigation of ketamine and dexmedetomidine in feed (사료 내 케타민과 덱스메데토미딘의 잔류조사를 위한 동시분석법 개발)

  • Chae, Hyun-young;Park, Hyejin;Seo, Hyung-Ju;Jang, Su-nyeong;Lee, Seung Hwa;Jeong, Min-Hee;Cho, Hyunjeong;Hong, Seong-Hee;Na, Tae Woong
    • Analytical Science and Technology
    • /
    • v.35 no.3
    • /
    • pp.136-142
    • /
    • 2022
  • According to media reports, the carcasses of euthanized abandoned dogs were processed at high temperature and pressure to make powder, and then used as feed materials (meat and bone meal), raising the possibility of residuals in the feed of the anesthetic ketamine and dexmedetomidine used for euthanasia. Therefore, a simultaneous analysis method using QuEChERS combined with high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry was developed for rapid residue analysis. The method developed in this study exhibited linearity of 0.999 and higher. Selectivity was evaluated by analyzing blank and spiked samples at the limit of quantification. The MRM chromatograms of blank samples were compared with those of spiked samples with the analyte, and there were no interferences at the respective retention times of ketamine and dexmedetomidine. The detection and quantitation limits of the instrument were 0.6 ㎍/L and 2 ㎍/L, respectively. The limit of quantitation for the method was 10 ㎍/kg. The results of the recovery test on meat and bone meal, meat meal, and pet food showed ketamine in the range of 80.48-98.63 % with less than 5.00 % RSD, and dexmedetomidine in the range of 72.75-93.00 % with less than 4.83 % RSD. As a result of collecting and analyzing six feeds, such as meat and bone meal, prepared at the time the raw material was distributed, 10.8 ㎍/kg of ketamine was detected in one sample of meat and bone meal, while dexmedetomidine was found to have a concentration below the limit of quantitation. It was confirmed that the detected sample was distributed before the safety issue was known, and thereafter, all the meat and bone meal made with the carcasses of euthanized abandoned dogs was recalled and completely discarded. To ensure the safety of the meat and bone meal, 32 samples of the meat and bone meal as well as compound feed were collected, and additional residue investigations were conducted for ketamine and dexmedetomidine. As a result of the analysis, no component was detected. However, through this investigation, it was confirmed that some animal drugs, such as anesthetics, can remain without decomposition even at high temperature and pressure; therefore, there is a need for further investigation of other potentially hazardous substances not controlled in the feed.

Risk Assessment of Heavy Metals Migrated from Plastic Food Utensils, Containers, and Packaging Distributed in Korea (국내 유통 식품용 플라스틱 기구 및 용기, 포장의 중금속 위해도 평가)

  • Kyung Youn, Lee;Hyung Soo, Kim;Dae Yong, Jang;Ye Ji, Koo;Seung Ha, Lee;Hye Bin, Yeo;Ji Su, Yoon;Kyung-Min, Lim;Jaeyun, Choi
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
    • /
    • v.28 no.3
    • /
    • pp.175-182
    • /
    • 2022
  • Heavy metals can be intentionally or unintentionally introduced into plastic food utensils, containers, and packaging (PFUCP) as additives or contaminants, which can be ingested with food by humans. Here, seven-heavy metals (lead, cadmium, nickel, chromium, antimony, copper, and manganese) with toxicity concerns were selected, and risk assessment was done by establishing their migration from 137 PFUCP products made of 16 materials distributed in Korea. Migration of heavy metals was examined by applying 4% acetic acid as a food simulant (70℃, 30 minutes) to the PFUCP products. Inductively coupled plasma mass spectrometry (ICP-MS) was employed for the analysis of migrated heavy metals, and the reliability of quantitative results was confirmed by checking linearity, LOD, LOQ, recovery, precision, and expanded uncertainty. As a result of monitoring, heavy metals were detected at a level of non-detection to 8.76 ± 11.87 ㎍/L and most of the heavy metals investigated were only detected at trace amounts of less than 1 ㎍/L on average. However, antimony migrated from PET products was significantly higher than other groups. Risk assessment revealed that all the heavy metals investigated were safe with a margin of exposure above 311. Collectively, we demonstrated that heavy metals migrated from PFUCP products distributed in Korea appear to be within the safe range.

Improvement of an Analytical Method for Methoprene in Livestock Products using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 살충제 메토프렌의 잔류분석법 개선)

  • Park, Eun-Ji;Kim, Nam Young;Park, So-Ra;Lee, Jung Mi;Jung, Yong Hyun;Yoon, Hae Jung
    • Journal of Food Hygiene and Safety
    • /
    • v.37 no.3
    • /
    • pp.136-142
    • /
    • 2022
  • The research aims to develop a rapid and easy analytical method for methoprene using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A simple, highly sensitive, and specific analytical method for the determination of methoprene in livestock products (beef, pork, chicken, milk, eggs, and fat) was developed. Methoprene was effectively extracted with 1% acetic acid in acetonitrile and acetone (1:1), followed by the addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate. Subsequently, the lipids in the livestock sample were extracted by freezing them at -20℃. The extracts were cleaned using MgSO4, primary secondary amine (PSA), and octadecyl (C18), which were then centrifuged to separate the supernatant. Nitrogen gas was used to evaporate the supernatant, which was then dissolved in methanol. The matrix-matched calibration curves were constructed using 8 levels (1, 2.5, 5, 10, 25, 50, 100, 150 ng/mL) and the coefficient of determination (R2) was above 0.9964. Average recoveries spiked at three levels (0.01, 0.1, and 0.5 mg/kg), and ranged from 79.5-105.1%, with relative standard deviations (RSDs) smaller than 14.2%, as required by the Codex guideline (CODEX CAC/GL 40). This study could be useful for residue safety management in livestock products.

Monitoring of Residual Pesticides and Exposure Assessment of Olive Oil Products Sold on the Market (올리브유의 잔류농약 모니터링 및 노출량 조사)

  • Mi-Hui Son;Jae-Kwan Kim;You-Jin Lee;Ji-Eun Kim;Eun-Jin Baek;Byeong-Tae Kim;Seong-Nam Lee;Myoung-Ki Park;Yong-Bae Park
    • Journal of Food Hygiene and Safety
    • /
    • v.38 no.4
    • /
    • pp.211-216
    • /
    • 2023
  • A total of 100 commercially available olive oil products were analyzed for 179 pesticide residues using gas chromatography-tandem mass spectrometry (GC/MS/MS). The olive oil samples were mixed with organic solvents, centrifuged and frozen to remove fat, and pesticide residues were analyzed using the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) method. The determination coefficient (R2) of the analysis method used in this study was ≥0.998. The detection limit of the method ranged 0.004-0.006 mg/kg and its quantitative limit ranged 0.012-0.017 mg/kg. The recovery rate (n=5) measured at the level ranging 0.01-0.02, 0.1, and 0.5 mg/kg ranged 66.8-119.5%. The relative standard deviation (RSD) was determined to be ≤5.7%, confirming that this method was suitable for the "Guidelines for Standard Procedures for Preparing Food Test Methods". The results showed that a total of 151 pesticides (including difenoconazole, deltamethrin, oxyfluorfen, kresoxim-methyl, phosmet, pyrimethanil, tebuconazole, and trifloxystrobin) were detected in 64 of the 100 olive oil products. The detection range of these pesticide residues was 0.01-0.30 mg/kg. The percentage acceptable daily intake (%ADI) of the pesticides calculated using ADI and estimated daily intake (EDI) was 0.0001-0.1346, indicating that the detected pesticides were present at safe levels. This study provides basic data for securing the safety of olive oil products by monitoring pesticide residues in commercially available oilve oil products. Collectively, the analysis method used in this study can be used as a method to analyze residual pesticides in edible oils.

A Study on the Replacement of a Light Burnt Dolomite with a Waste MgO-C Refractory Material for a Steel-Making Flux in Electric Arc Furnace (폐 MgO-C계 내화재의 전기로(EAF) 제강 Flux용 경소돌로마이트 대체 사용 연구)

  • Hyun-Jong Kim;Jong-Deok Lim;Hang-Goo Kim;Jei-Pil Wang
    • Resources Recycling
    • /
    • v.31 no.6
    • /
    • pp.44-51
    • /
    • 2022
  • In the steelmaking process using an electric arc furnace (EAF), light-burnt dolomite, which is a flux containing MgO, is used to protect refractory materials and improve desulfurization ability. Furthermore, a recarburizing agent is added to reduce energy consumption via slag foaming and to induce the deoxidation effect. Herein, a waste MgO-C based refractory material was used to achieve the aforementioned effects economically. The waste MgO-C refractory materials contain a significant amount of MgO and graphite components; however, most of these materials are currently discarded instead of being recycled. The mass recycling of waste MgO-C refractory materials would be achievable if their applicability as a flux for steelmaking is proven. Therefore, experiments were performed using a target composition range similar to the commercial EAF slag composition. A pre-melted base slag was prepared by mixing SiO2, Al2O3, and FeO in an alumina crucible and heating at 1450℃ for 1 h or more. Subsequently, a mixed flux #2 (a mixture of light-burnt dolomite, waste MgO-C based refractory material, and limestone) was added to the prepared pre-melted base slag and a melting reaction test was performed. Injecting the pre-melted base slag with the flux facilitates the formation of the target EAF slag. These results were compared with that of mixed flux #1 (a mixture of light-burnt dolomite and limestone), which is a conventional steelmaking flux, and the possibility of replacement was evaluated. To obtain a reliable evaluation, characterization techniques like X-ray diffraction (XRD) analysis and X-ray fluorescence (XRF) spectrometry were used, and slag foam height, slag basicity, and Fe recovery were calculated.

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
    • /
    • v.55 no.4
    • /
    • pp.166-177
    • /
    • 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.

Physiological and Proteomic Responses of Barley Seedlings to Salt Stress (보리의 생육초기 염 스트레스에 따른 생리적 반응과 프로테옴 변화)

  • Kim, Dea-Wook;Yun, Seong-Kun;Park, Hyoung-Ho;Hwang, Jong-Jin;Han, Ok-Kyu;Park, Tae-Il;Jung, Gun-Ho;Lee, Jae-Eun;Kim, Sun-Lim;Chung, Young-Ho
    • Journal of the Korean Society of International Agriculture
    • /
    • v.23 no.5
    • /
    • pp.537-545
    • /
    • 2011
  • This study was conducted to obtain basic information on physiological and proteomic responses of barley seedlings to salt stress. Shoot dry weight decreased significantly as the level of soil salinity increased. Salt stress-induced decrease of relative shoot dry weight was lower in cv. "Sanglok" than in cv. "Sunwoo". Under the salt stress, SPAD value decreased, and the value was higher in cv. "Sanglok" than in cv. "Sunwoo". Sodium ion content in the leaves increased as NaCl concentration increased, and the content was higher in cv. "Sunwoo" than in cv. "Sanglok". The K+/Na+ ratio was higher in cv. "Sanglok" than in cv. "Sunwoo". Salt stress-induced alterations in protein expression of the leaves were detected by two dimensional electrophoresis, and 47 protein spots showing altered expression were selected. Among the selected protein spots, 17 protein spots were up-regulated and 28 spots down-regulated in cv. "Sanglok". In cv. "Sunwoo", 14 protein spots were up-regulated and 27 spots down-regulated. Out of 47 deferentially expressed protein spots, 18 protein spots were identified using mass spectrometry and NCBI protein database. Among the identified proteins, ten proteins are known to be involved in various stress responses, but the others are not directly involved in stress responses.

Applications of Radiocarbon Isotope Ratios in Environmental Sciences in South Korea (방사성탄소동위원소비 분석을 적용한 우리나라 환경과학 연구)

  • Neung-Hwan Oh;Ji-Yeon Cha
    • Korean Journal of Ecology and Environment
    • /
    • v.56 no.4
    • /
    • pp.281-302
    • /
    • 2023
  • Carbon is not only an essential element for life but also a key player in climate change. The radiocarbon (14C) analysis using accelerator mass spectrometry (AMS) is a powerful tool not only to understand the carbon cycle but also to track pollutants derived from fossil carbon, which have a distinct radiocarbon isotope ratio (Δ14C). Many studies have reported Δ14C of carbon compounds in streams, rivers, rain, snow, throughfall, fine particulate matter (PM2.5), and wastewater treatment plant effluents in South Korea, which are reviewed in this manuscript. In summary, (1) stream and river carbon in South Korea are largely derived from the chemical weathering of soils and rocks, and organic compounds in plants and soils, strongly influenced by precipitation, wastewater treatment effluents, agricultural land use, soil water, and groundwater. (2) Unprecedentedly high Δ14C of precipitation during winter has been reported, which can directly and indirectly influence stream and river carbon. Although we cannot exclude the possibility of local contamination sources of high Δ14C, the results suggest that stream dissolved organic carbon could be older than previously thought, warranting future studies. (3) The 14C analysis has also been applied to quantify the sources of forest throughfall and PM2.5, providing new insights. The 14C data on a variety of ecosystems will be valuable not only to track the pollutants derived from fossil carbon but also to improve our understanding of climate change and provide solutions.

The content and risk assessment of heavy metals in commercial herbal medicines (서울지역 유통한약재의 중금속 함량 및 위해성 평가)

  • Young Shin;Sang-Hun Park;Seung-Hye Han;So-Hyun Park;Ji-Hye Kim;Hyun-Jung Jang;Ae-Kyoung Kim;Ju-Seung Park
    • Analytical Science and Technology
    • /
    • v.36 no.6
    • /
    • pp.267-280
    • /
    • 2023
  • This study investigated the contents of Pb, Cd, As, and Hg for 4333 samples with 2 09 types of herbal medicines distributed in Seoul area from 2019 to 2021, and evaluated risk assessment according to medicinal part used and origin. The contents of heavy metals were analyzed by inductively coupled plasma mass spectrometry (ICP-MS) and mercury analyzer. The average contents (mg/kg) of heavy metals by medicinal parts were 0.123 to 1.290 for Pb, 0.018 to 0.131 for Cd, 0.034 to 0.290 for As, and 0.003 to 0.015 for Hg. The contents of Pb were higher in Leaves and Whole Herbs (above-ground part) than underground part (Radix & Rhizoma) (ANOVA-test, p < 0.05). The contents of Cd were high in Leaves, Radix & Rhizoma, and Stems & Woods (ANOVA-test, p <0 .05), and exceeded regulatory limits in various types. Levels of Pb, Cd concentrations exceeding regulatory limits were observed in 8, 22 samples (8, 14 types). No sample exceeded regulatory limits of As and Hg. In the comparison between countries of origin, the contents of Cd, As, and Hg were high in imported herbal medicines (t-test, p < 0.05). As a result of the risk assessment, except for Thujae Orientalis Folium and Spirodelae Herba, the MOE values of Pb were all 1 or more, and most samples were safe. The Hazard Index (HI) for Cd, As, and Hg were evaluated to be less than 100 % even if the risk (%) of each heavy metal was added, and the risk from taking herbal medicines was evaluated to be safe.

Development of a Simultaneous Analytical Method for Azocyclotin, Cyhexatin, and Fenbutatin Oxide Detection in Livestock Products using the LC-MS/MS (LC-MS/MS를 이용한 축산물 중 유기주석계 농약 Azocyclotin, Cyhexatin 및 Fenbutatin oxide의 동시시험법 개발)

  • Nam Young Kim;Eun-Ji Park;So-Ra Park;Jung Mi Lee;Yong Hyun Jung;Hae Jung Yoon
    • Journal of Food Hygiene and Safety
    • /
    • v.38 no.5
    • /
    • pp.361-372
    • /
    • 2023
  • Organotin pesticide is used as an acaricide in agriculture and may contaminate livestock products. This study aims to develop a rapid and straightforward analytical method for detecting organotin pesticides, specifically azocyclotin, cyhexatin, and fenbutatin oxide, in various livestock products, including beef, pork, chicken, egg, and milk, using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The extraction process involved the use of 1% acetic acid in a mixture of acetonitrile and ethyl acetate (1:1). This was followed by the addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium chloride. The extracts were subsequently purified using octadecyl (C18) and primary secondary amine (PSA), after which the supernatant was evaporated. Organotin pesticide recovery ranged from 75.7 to 115.3%, with a coefficient of variation (CV) below 25.3%. The results meet the criteria range of the Codex guidelines (CODEX CAC/GL 40). The analytical method in this study will be invaluable for the analysis of organotin pesticides in livestock products.