• 제목/요약/키워드: Mass Spectrometer

검색결과 728건 처리시간 0.03초

A Study on Heavy Metal and Selenium Levels in Dried Seafoods (건조수산물의 중금속 및 셀레늄 함량)

  • Kwon, Hye-Jung;Kim, Ki-Cheol;Kim, Kyung-A;Kim, Young-Su;Kang, Suk-Ho;Kwak, Shin-Hye;Kang, Kyung-Ja;Lee, Pil-Suk;Cho, Wook-Hyun;Moh, Ara;Park, Yong-Bae
    • Journal of Food Hygiene and Safety
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    • 제34권6호
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    • pp.562-570
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    • 2019
  • The heavy metal concentrations in dried seafoods commonly consumed in Gyeonggi-do were analyzed. Concentrations of lead (Pb), cadmium (Cd), mercury (Hg) and selenium (Se) were measured in 95 samples with an inductively-coupled plasma-mass spectrometer (ICP-MS) and an Hg analyzer. The average concentration [mean±SD(minimum-maximum) mg/kg] of heavy metals were as follows: Pb 0.062±0.071(0.002-0.428), Cd 0.083±0.100(0.004-0.540), Hg 0.012±0.012(N.D-0.054) and Se 0.839±0.371(0.362-2.124). All the levels were below the recommended standards of the MFDS (Ministry of Food and Drug Safety). In the comparison of heavy metal content by anchovy size, it was shown that mercury was significantly higher in large anchovy (P<0.05). Selenium levels were found to differ significantly in small anchovy and large anchovy (P<0.05). Pb, Cd and Hg were significantly higher in Tiger prawn among shrimp (P<0.05). The heavy metal and selenium levels of anchovy and shad were highest in the intestine. However, the heavy metal and selenium levels of shrimp were highest in the head. In addition, weekly (monthly) intake of mercury and cadmium from dried seafoods was found to be 0.712% and 2.978% of PTW(M)I (Provisional Tolerable Weekly(Monthly) Intake) respectively. Therefore, it was found that dried seafoods were safe for consumption.

Development of an Analytical Method for Fluxapyroxad Determination in Agricultural Commodities by HPLC-UVD (HPLC-UVD를 이용한 농산물 중 Fluxapyroxad 잔류분석법 개발)

  • Kwon, Ji-Eun;Kim, HeeJung;Do, Jung-Ah;Park, Hyejin;Yoon, Ji-Young;Lee, Ji-Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • 제29권3호
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    • pp.234-240
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    • 2014
  • Fluxapyroxad is classified as carboxamide fungicide that inhibits succinate dehydrogenase in complex II of mitochondrial respiratory chain, which results in inhibition of mycelial growth within the fungus target species. This study was carried out to assure the safety of fluxapyroxad residues in agricultural products by developing an official analytical method. A new, reliable analytical method was developed and validated using High Performance liquid Chromatograph-UV/visible detector (HPLC-UVD) for the determination of fluxapyroxad residues. The fluxapyroxad residues in samples were extracted with acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient($R^2$) of fluxapyroxad standard solution was 0.9999. The method was validated using apple, pear, peanut, pepper, hulled rice, potato, and soybean spiked with fluxapyroxad at 0.05 and 0.5 mg/kg. Average recoveries were 80.6~114.0% with relative standard deviation less than 10%, and limit of detection (LOD) and limit of quantification (LOQ) were 0.01 and 0.05 mg/kg, respectively. All validation parameters were followed with Codex guideline (CAC/GL 40). LC-MS (Liquid Chromatograph-Mass Spectrometer) was also applied to confirm the analytical method. Base on these results, this method was found to be appropriate fluxapyroxad residue determination and can be used as the official method of analysis.

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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    • 제30권1호
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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.

A Study on the Identification of Animal Hair in Food (식품 중 동물 털 이물의 판별법 연구)

  • Lee, Jae-Hwang;Park, Young-Eun;Lim, Byung-Chul;Kim, Ju-Shin;Choi, Jong-Hyun;Kang, Tae Sun;Lee, Jin-Ha;Kwon, Kisung
    • Journal of Food Hygiene and Safety
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    • 제32권1호
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    • pp.57-63
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    • 2017
  • Foreign materials with a variety of types and sizes are found in food; thus, extraordinary efforts and various analytical methods are required to identify the types of foreign materials and to find out accurate causes of how they unintentionally enter food. In this study, human, cow, pig, mouse, duck, goose, dog, and cat were chosen as various types of animal hairs because they can be frequently incorporated into food during its production or consumption step. We morphologically analyzed them using stereoscopic, optical, SUMP method, and scanning electron microscopes, showing differences in each type. In addition, X-ray fluorescence spectrometer (XRF) was used to analysis chemical compositions ($^{11}Na{\sim}^{92}U$, Mass%) of samples. As a result, we observed that mammalian hairs were mainly composed of sulfur. Organic compounds of samples were further analyzed by fourier transform infrared spectroscopy (FT-IR) that can compare spectra of given materials; however, this method did not show significant differences in each sample. In this study, we suggest a rapid method for the identification of the causes and types of foreign materials in food.

Ethyl acetate fraction from Pteridium aquilinum ameliorates cognitive impairment in high-fat diet-induced diabetic mice (고지방 식이로 유도된 실험동물의 당뇨성 인지기능 장애에 대한 고사리 아세트산에틸 분획물의 개선효과)

  • Kwon, Bong Seok;Guo, Tian Jiao;Park, Seon Kyeong;Kim, Jong Min;Kang, Jin Yong;Park, Sang Hyun;Kang, Jeong Eun;Lee, Chang Jun;Lee, Uk;Heo, Ho Jin
    • Korean Journal of Food Science and Technology
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    • 제49권6호
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    • pp.649-658
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    • 2017
  • The potential of the ethyl acetate fraction from Pteridium aquilinum (EFPA) to improve the cognitive function in high-fat diet (HFD)-induced diabetic mice was investigated. EFPA-treatment resulted in a significant improvement in the spatial, learning, and memory abilities compared to the HFD group in behavioral tests, including the Y-maze, passive avoidance, and Morris water maze. The diabetic symptoms of the EFPA-treated groups, such as fasting glucose and glucose tolerance, were alleviated. The administration of EFPA reduced the acetylcholinesterase (AChE) activity and malondialdehyde (MDA) content in mice brains, but increased the acetylcholine (ACh) and superoxide dismutase (SOD) levels. Finally, kaempferol-3-o-glucoside, a major physiological component of EFPA, was identified by using high-performance liquid chromatography coupled with a hybrid triple quadrupole-linear ion trap mass spectrometer (QTRAP LC-MS/MS).

Development of analytical method for determination of spinetoram residues in livestock using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 Spinetoram 공정시험법 개발 및 검증)

  • Ko, Ah-Young;Kim, Heejung;Do, Jung Ah;Jang, Jin;Lee, Eun Hyang;Ju, Yun Ji;Kim, Ji Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Analytical Science and Technology
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    • 제29권2호
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    • pp.94-103
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    • 2016
  • An analytical method was developed to determine the amount of spinetoram (spinetoram J and spinetoram L) in livestock samples. The spinetoram was extracted with acetonitrile and purified through a primary secondary amine (PSA) sorbent. The spinetoram residues were then quantified and confirmed using a liquid chromatography–tandem mass spectrometer (LC-MS/MS) in the positive ion mode using multiple reactions monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/kg) into a blank extract with r2 > 0.994. The limits of detection and quantification were 0.002 and 0.01 mg/kg, respectively. The recovery results of spinetram ranged between 81.9-106.4% at different concentration levels (LOQ, 10LOQ, 50LOQ, n=5) with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003). An interlaboratory study was conducted to validate the method. The proposed analytical method proved to be accurate, effective, and sensitive for spinetoram determination. The method will be used as an official analytical method in Korea.

A comparative analysis of gas and liquid phase standard spiked solid sorbent tubes for the determination of volatile organic compounds in indoor air by TD-GC/MS (열탈착/저온농축-GC/MS에 의한 실내공기 중 휘발성 유기화합물 정량용 기체상 및 액체상 표준물질 첨가한 고체 흡착관의 비교 분석)

  • Lim, Hyun-Woo;Jung, Sung-Won;Kang, Chul-Ho;Park, Jin-Sook;Park, Byeong Moo;Choi, Yong-Wook
    • Analytical Science and Technology
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    • 제26권4호
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    • pp.287-297
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    • 2013
  • The optimization of analytical method for the thermal desorption of seven VOCs (volatile organic compounds) by TD-GC/MS (thermal desorption-gas chromatograph-mass spectrometer) with solid phase sorbent tube, and comparative analysis for the determination of VOCs plotted by standard sorbent tubes prepared using both gas phase and liquid phase materials were investigated. The result of paired t-test showed that a liquid phase standard sorbent tube method was in agreement with a gas phase standard sorbent tube method for six species of VOCs including benzene, toluene, ethylbenzene, o-, m-, and p-xylene except for styrene at the significance level (${\alpha}=0.01$), while the 15.6% of difference in response factor between both of gas phase and liquid phase standard plotting for the determination of styrene showed that both methods were significantly different at the significance level. Therefore, the liquid phase standard plotting method was employed to reduce erroneous data for the determination of styrene including BTEX. Under the optimized analytical method by liquid phase standard sorbent tube, recovery was between $100{\pm}5%$ for 7 species of VOCs, reproducibility ranged from 0.3 to 7.7%, and method detection limit (MDL) ranged from $0.01{\mu}g/m^3$ for o-xylene to $0.27{\mu}g/m^3$ for toluene. The optimized standard method was applied to determine VOCs VOCs from indoor air of of dormitory, one bedroom apartment, and a new car.

Development of Simultaneous Analytical Method for Determination of Isoxaflutole and its Metabolite (Diketonitrile) residues in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Isoxaflutole과 대사산물(Diketonitrile)의 동시시험법 개발)

  • Ko, Ah-Young;Kim, Heejung;Do, Jung Ah;Jang, Jin;Lee, Eun-Hyang;Ju, Yunji;Kim, Ji Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • The Korean Journal of Pesticide Science
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    • 제20권2호
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    • pp.93-103
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    • 2016
  • A simultaneous analytical method was developed for the determination of isoxaflutole and metabolite (diketonitrile) in agricultural commodities. Samples were extracted with 0.1% acetic acid in water/acetonitrile (2/8, v/v) and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2 by 1 N hydrochloric acid. The analytes were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive-ion mode using multiple reaction monitoring (MRM). Matrix matched calibration curves were linear over the calibration ranges ($0.02-2.0{\mu}g/mL$) for all the analytes into blank extract with $r^2$ > 0.997. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries were ranged between 72.9 to 107.3%, with relative standard deviations (RSDs) less than 10% for all analytes. All values were consistent with the criteria ranges requested in the Codex guideline (CAC/GL40, 2003). Furthermore, inter-laboratory study was conducted to validate the method. The proposed analytical method was accurate, effective, and sensitive for isoxaflutole and diketonitrile determination in agricultural commodities.

A study on the fixation of heavy metals with modified soils in the landfill liner (개량혼합토를 이용한 폐기물 매립지 차수층의 중금속 고정능력에 관한 연구)

  • 노회정;이재영
    • Journal of Soil and Groundwater Environment
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    • 제7권2호
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    • pp.63-71
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    • 2002
  • The authors selected the modified soil method, and then performed the geotechnical and environmental laboratory test, and evaluated whether the modified soil liner could be accepted as a barrier layer in landfill. Unlike the results of the natural soil(CL), those of the hydraulic conductivity test of stabilized soil met the standard value. According to these results, the optimal mixing ratio of a mixture(cement : bentonite : stabilizing agent) was 90 : 60 : 1 with mass ratio(kg) for 1㎥ with soil, and it was possible to use poor quality bentonite. B\circled2 because of a little difference from results with high quality bentonite. B\circled1. The Cation Exchange Capacity(CEC) of the modified soil was increased about 1.5 times compared with the natural soil; however. the change of CEC with a sort of additives was not detected. In order to observe the change of the chemical components and crystal structures, the natural and the modified soils with the sorts of additives were measured by the XRF(X-Ray Flourescence Spectrometer) and SEM, but there was no significant change. The artificial leachate with the heavy meals ($Pb^{2+}$ , $Cu^{2+}$, $Cd^{2+}$ Zn$^{2+}$ 100mg/L) was passed through the natural soil and modified soils in columns. In the natural soil, Cd$^{2+}$ and $Zn^{2+}$ were identified, simultaneously the pH of outflow was lower, and then came to the breakthrough point. The removal efficiency of the natural soil was showed in order of following : $Pb^{2+}$$Cu^{2+}$ > $Zn^{2+}$ > $Cd^{2+}$ On the other hand, modified soils were not showed the breakthrough condition like the result of the natural soil. The modified soil with the lower quality bentonite, B\circled2(column3) was more stable with respect to chemical attack than that with the higher bentonite, B\circled1(column2) because the change range of outflow pH in columns was less than that of outflow pH in column2. In addition, the case of adding the stabilizing agent(column4) was markedly showed the phenomena.ena.

Establishment of an Analytical Method for Determination of Fungicide Oxathiapiprolin in Agricultural Commodities using HPLC-UV Detector (HPLC-UVD를 이용한 농산물 중 살균제 Oxathiapiprolin의 잔류분석법 확립)

  • Jang, Jin;Kim, Heejung;Do, Jung Ah;Ko, Ah-Young;Lee, Eun Hyang;Ju, Yunji;Kim, Eunju;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • 제31권3호
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    • pp.186-193
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    • 2016
  • An analytical method was developed for the determination of oxathiapiprolin in agricultural commodities. Oxathiapiprolin is a new oomycide (fungicide of piperidinyl thiazole isoxazoline class) which controls downy mildew in cucurbits caused by Pseudoperonospora cubensis (oomycete plant pathogen). Agricultural commodities were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, adjusting pH between 9 and 10 by 1 N sodium hydroxide. After purification by silica SPE cartridge to clean up the interference of organic compounds, they were finally quantified by HPLC-UVD (high performance liquid chromatograph ultraviolet detector) using a wavelength at 260 nm and confirmed by LC-MS (liquid chromatograph mass spectrometer) in electro-spray ionization positive ion mode. The standard calibration curve was linear with coefficients of determination ($r^2$) 1.00 over the calibration ranges (0.025-2.5 mg/L). Recoveries were ranged between 86.7 to 112.7%, with relative standard deviations less than 10% at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates. The overall results were determined and estimated according to the CODEX guidelines (CAC/GL40). The proposed method for determination of oxathiapiprolin residues in agricultural commodities can be used as an official method.