• 제목/요약/키워드: GC and GC/MSD analysis

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ASE 및 SPE 복합정제법을 이용한 친환경농업토양의 다성분잔류농약 분석 (Pesticide Multiresidues Analysis of Environmental-friendly Agricultural Soils by the Complex Cleanup Method of Accelerated Solvent Extraction (ASE) and Solid Phase Extraction (SPE))

  • 문경미;박진우;이영근;최영환
    • 농업생명과학연구
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    • 제45권5호
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    • pp.73-80
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    • 2011
  • 국내의 친환경농산물과 토양에서 자주 검출되는 농약 50성분을 선정하고, 경남지역의 친환경농산물 재배농지의 토양시료 40점을 대상으로, 가속용매추출법(accelerated solvent extraction)과 고상추출법(solid-phase extraction)의 복합처리법으로 정제하고 GC/ECD/NPD, HPLC/UV/FL, GC/MSD 및 HPLC/MSD를 이용한 분석법을 적용하여 잔류농약의 잔류실태를 조사하였다. 적용한 분석법에 의한 농약 회수율은 72~118%의 범위로 평균 95.5%이었고, CV(%)값 평균은 3.0%로 나타났다. 토양 40점 중 잔류농약 검출은 21점에서 20성분이 검출되었으며 검출토양의 농약별평균 검출량은 endosulfan 0.035, ethoprophos 0.043, chlorpyrifos 0.020, chlorfenapyr 0.023, flufenoxuron 0.047, fenvalerate 0.070, cypermethrin 0.266, lufenuron 0.016, bifenthrin 0.022, fenobucarb/BPMC 0.025, difenoconazole 0.043, fenarimol 0.059, kresoxim-methyl 0.020, tetraconazole 0.026, isoprothiolane 0.039, iprobenfos 0.017, nuarimol 0.014, fluquinconazole 0.156, tebuconazole 0.047 및 oxadiazon이 0.045 mg/kg으로 나타나서 친환경재배농지의 토양환경기준에 잔류농약의 설정이 시급하다고 판단되었다.

작업장 공기 중 파라티온과 작업자 소변 중 p-니트로페놀의 시료채취 및 분석 (Sampling and Analysis of Parathion in the Air and Urinary p-Nitrophenol for Parathion Manufacturing Workers)

  • 한돈희
    • 한국산업보건학회지
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    • 제17권4호
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    • pp.300-309
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    • 2007
  • Although parathion is an organophosphate pesticide being legally applied for the purpose of agriculture and is being manufactured, parathion in the air and urinary p-nitrophenol, a metabolite of parathion, were not analysed in Korea. Air of the parathion manufacturing workplace was sampled by OVS-2 tubes using NIOSH 5600 and spot urine of workers was sampled at the end of shift. Parathion and urinary p-nitrophenol were analysed by GC/MS (5973 MSD connected with Agilent 6890 GC) and the protocol was included in this study. It was found that this protocol should be so sensitive that determining parathion in the air and urinary p-nitrophenol below level of ACGIH TLV and BEI be adequate. Another finding was that total sampling volume of air of NIOSH 5600 of 240 L should be adjusted to be less than 120 L due to breakthrough.

손소독제 사용 실태 조사 및 성분 분석 (Survey on the Use of Hand Sanitizer and Component Analysis)

  • 윤혜경;이은지;허예림;박나연;고영림
    • 한국환경보건학회지
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    • 제46권6호
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    • pp.702-709
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    • 2020
  • Objectives: Hand sanitizer is made with ethyl alcohol as the main ingredient. Problems related to the use of hand sanitizers and cases of harm caused by the use of hand sanitizers are occurring. This study investigated the usage behavior and recognition level of people using hand sanitizer and identified the chemical components listed in the component label of hand sanitizer. In addition, the methanol and isopropanol contained in hand sanitizer were quantified using HS-GC-MSD. Methods: The investigation of the behavior and recognition of hand sanitizer usage was conducted through a survey of 143 college students and adults. The components marked on 34 types of hand sanitizers were investigated, and methanol and isopropanol concentrations were analyzed using the HS-GC-MSD method. Results: According to the survey, 57% of respondents use hand sanitizers two to three times per day, 92.3% of them do so when in public places and 41.3% of them do so at home. Ethanol, purified water, carbomer, glycerin, and triethanolamine were the ingredients listed in the hand sanitizer. Among the 34 samples, methanol and isopropyl alcohol were detected in 33 samples, the concentration range for methanol was ND-567 ppm, and the concentration range of isopropyl alcohol was ND-2121 ppm. Conclusion: The results of this study have shown that hand sanitizers are being used constantly every day, and methanol, which is not included in the marked content, was detected in a significant concentration compared to wet tissue. It has been found that maintenance of hand sanitizer manufacturing standards and training on how to use them are needed.

Detection and Quantitation of Residual Antibiotics and Antibacterial Agents in Foods

  • Ryu, Jae-Chun;Seo, Ja-Won;Song, Yun-Seon;Park, Jong-Sei
    • 한국식품위생안전성학회지
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    • 제5권3호
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    • pp.159-164
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    • 1990
  • To detect and quantitation residual antibiotics and antibacterial agents in meats, we performed a biological assay employing the three microorganisms Bacillus subtilis ATCC 6633, Micrococcus luteus ATCC 9341, and Bacillus cereus var. mycoides ATCC 11778 for the screening purpose and developed a Gas Chromatography-mass Spectrometry(GC/MS) analysis for the confirmation and quantiation. In the biological assay (paper disk method), three test solution are used depending on the character of the residual antibiotics and antibacterial agents, follow by a simple clean up procedure which includes homogenization with Mcilvaine buffer, defatting with includes homogenization with Mcilvaine buffer, defatting with hexane, extraction with chloroform, clean-up by Sep-Pak $C_{18}$ and Bakerbond SPE carboxylic acid column. The chloroform layer is used for the analysis of sulfa agents. macrolides antibiotics and antibacterial agents, Adsorbed materials in the Sep-Pak $C_{18}$ were also employed for th analysis of penicillins and tetracyclines. Effluents from the Sep-Pak $C_{18}$ were cleaned-up one more by Bakerbond 10 SPE COOH column and employed for the analysis of aminoglycosides. In the instrumental analysis by using the GC/MSD, residual antibiotics and antibacterial agent were quantitated by selected ion monitoring (SIM) mode after derivatization. A simultaneous analysis of six residual antibiotic and antibacterial agent such as oxytetracycline, penicillin, ampicillin, choliraphenicol and thiamphenicol was developed with simple cleanup procedures revealing good recovery and reproducibility. Also, simultaneous detection of macrolides antibiotics such as erythromycin, spiramycin, and oleandomycin was developed after acid hydrolysis due to their large molecular structures. Because of the high reproducibility and selectivity of these two methods, it is very desirable that the combination of the two methods be used in the bioassay for the screening of residual antibiotics and antibacterial agent and that GC/MSD analysis be used for the confirmation and quantitation.

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천연 강황 추출물의 약리, 화학적 특성 및 분석 (A Study on the Pharmaceutical & Chemical Characteristics and Analysis of Natural Curcumin Extract)

  • 성기천
    • 한국응용과학기술학회지
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    • 제28권4호
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    • pp.393-401
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    • 2011
  • Natural Curcumin belongs to Zingiber Officinale Roscoe was known to possess natural odor, natural taste, natural color, and other pharmaceutical & chemical characteristics. Natural Curcumin extract was made to use ethanol as a solvent was to show a yellow color having state of solid powder and an active component. Natural Curcumin extract tested pharmaceutical & chemical experiment to dilute in curcumin 1%-water solution. Curcumin extract tested antimicrobial experiment using microbe, and tested dye experiment using fiber. Some conclusions in the result of characteristics experiment was obtained as follow. The result of antimicrobial experiment showed that the growth of staphylococcus aureus (ATCC-001) and aspergillus niger (ATCC-002) as microbes decreased according to passage of time. This phenomenon could know that Curcumin compoment showed influence to antimicrobial effect. Also, the result of dye experiment showed that cotton and sick with fiber dyeing dyed in direction of dark yellow color. This phenomenon could know that Curcumin extract showed influence to dyeing effect in observation of optical electron microscope(OEM.) The result of instrument analysis ascertained inorganic components of K(53.300ppm), Na(1.150ppm), Ca(0.711ppm), Ti(0.351ppm), Li(0.256ppm), Cu(0.233ppm) etcs from Curcumin component with ICP/OES, and ascertained organic components of propanoic acid(1.859), benzene(10.814), phenol(14.194) etcs from Curcumin component with GC/MSD.

부·울·경에서 판매되는 도료 희석제의 구성성분 함량과 물질안전보건자료의 신뢰성에 관한 연구 (Benzene Contents and Reliability of Material Safety Data Sheets for Paint Thinners sold in Busan, Ulsan, and Gyeongnam)

  • 우성준;하권철
    • 한국산업보건학회지
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    • 제32권4호
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    • pp.340-349
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    • 2022
  • Objectives: The importance of MSDS is emphasized for communicating hazardous information due to the increase in the types and usage of chemical substances. The purpose of this study is to assess the reliability of MSDS by collecting and examining paint thinners commercially available in South Korea. Methods: Twenty-five paint thinners were purchased at paint stores and the provision of MSDS was checked. Quantitative and qualitative analysis was performed on the chemical constituents of the thinners using GC-MSD and GC-FID. Reliability was evaluated by the MSDS collection rate for the paint thinners and calculating the rate of matching between laboratory analysis results and the contents and composition of chemical constituents given in the MSDS. Results: Unlike a study conducted in 2006, MSDS were provided for all 25 thinners. As a result of qualitative analysis using GC-MSD, 104 chemical substances were detected. The substances with the highest detection rate were identified in the order of toluene, butyl acetate, acetone, xylene, and ethyl benzene. A component matching rate of 41% was found by comparing the differences between the number of substances detected in laboratory testing and the number of substances listed in the MSDS. Benzene, a carcinogen not listed in the MSDS, was detected in two thinners produced by a small company. The detected benzene contents were 0.039 and 0.040%. When benzene is used, it should be strictly handled according to the Industrial Safety and Health Act. However, since it is not listed on the MSDS, it is judged that benzene was not being managed as a carcinogen in the workplaces where it is used. Conclusions: Since the reliability of MSDS, which play an important role in hazard communication, was evaluated to be low, it is necessary to systematically and continuously secure this reliability. In particular, carcinogens should be managed more strictly.

열탁착식 가스크로마토질량분석기에 의한 국내 산지별 백리향의 휘발성향기성분 (Volatile Aroma Compounds of Several Domestic Thymus quinquecostatus by Thermal Desorption Gas Chromatograph Mass Spectrometer)

  • 장매희;이광우;백정애
    • 생물환경조절학회지
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    • 제20권1호
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    • pp.14-20
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    • 2011
  • 지역별로 자생하고 있는 백리향 지상부의 휘발성 향기 성분 및 방부성 물질인 phenols의 성분을 조사하기 위해 제주도 고산종, 제주도 중간산종, 경기도, 울릉도, 강원도 서식종을 TD-GC-MSD로 분석한 결과 제주도 중간산종에서 상대적으로 높은 62종의 물질이 조사되었으며 함량도 $7365.22{\mu}g/m^3$으로 높은 농도를 나타냈다. 또한 백리향의 휘발성 향기성분 중 제주도 중간산종이 다른 조사지역보다 상대적으로 thymol과 carvacrol의 phenol성 물질이 다른 휘발성분에 비해 35.92%로 높은 결과를 보였다.

Microcystis sp.의 오존접촉특성 및 부산물 생성에 관한 연구 (Investigation on the products generated by the ozonation of Microcystis sp.)

  • 김영웅;손희종;유명호;이춘식;김성윤
    • 한국물환경학회지
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    • 제16권4호
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    • pp.479-490
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    • 2000
  • This study investigated the removal characteristics, Microcystin decomposition and generation of by-products when aqueous Microcystis sp. is oxidized by ozone. The concentration of Microcystin (MC) in aqueous solution has been found by HPLC analysis to decrease continuously by ozonation after the initial, abrupt increase. The kinetic constant of the decomposition of MC-RR and -LR were 0.0596 and 0.0243, respectively. This means that removal efficiency of MC-RR by its oxidative decomposition is preferable compared with that of MC-LR. On the other hand, it has been found that the decomposition product, TOC, exhibits the continuous decrease in the concentration by further ozonation, while DOC and UV-254 increase temporarily until 10 minutes before the decrease. Furthermore, the GC/MSD analysis has revealed that the ozonation of Microcystis sp. for 100minutes affords five kinds of aldehydes, six kinds of alcohols, and trans-1, 2-dimethyl-cyclopropane.

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GC/ECD와 GC/MS를 이용한 농산물 중 Picoxystrobin의 분석법 개발 (Development of Analytical Method for Picoxystrobin in Agricultural Commodities Using GC/ECD and GC/MS)

  • 권혜영;김찬섭;박병준;김일환;홍수명;손경애;진용덕;이제봉;임건재;김두호
    • 한국환경농학회지
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    • 제31권2호
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    • pp.146-151
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    • 2012
  • BACKGROUND: This study was conducted to develop analytical method for picoxystrobin in agricultural commodities using GC/ECD and GC/MS. METHODS AND RESULTS: Each steps of analytical method were optimized for determining picoxystrobin residues in various agricultural commodities. The developed methods include acetone extraction, n-hexane/saline water partition and florisil column chromatography for analysis of all samples (apple, potato, green pepper, hulled rice and soybean), and in addition to these steps, solid phase extraction (SPE) was used for analysis of green pepper and n-hexane/acetonitrile partition was used for analysis of hulled rice and soybean. The instrumental conditions were tested for quantitation in GC/ECD and for confirmation in GC/MS. Recovery was in the range of 86~109% with RSD ${\leq}$10.2% and the quantitation limits (LOQ) of method were 0.025 mg/kg in all agricultural commodities. CONCLUSION: The result showed that the developed method can be used to determine picoxystrobin residue in agricultural commodities.

흡착 열탈착 장치와 GC/MS를 이용한 휘발성 유기화합물의 분석과 악취원인 성분의 예측 - 음식물 퇴비화 과정에서 발생되는 악취분석의 예 - (Analysis of Volatile Organic Compounds by GC/MS with the Thermal Desorber and Characterization of the Major Components Attributing to Malodor -An Analytical Example of the Odor Emitted from the Compost of Food Waste-)

  • 유미선;양성봉;안정수
    • 분석과학
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    • 제15권1호
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    • pp.80-86
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    • 2002
  • 흡착/열탈착/GC/MS를 이용하여 우리나라와 일본의 법정 악취성분을 한 컬럼으로 동시분석이 가능한가를 검토하였다. 트리메틸아민, 아세트알데히드, 메틸메르캅탄, 이메틸황 은 대략적인 농도를 추정할 수 있었으며, 스티렌, 이황화메틸, 이황화이메틸 그리고 프로피온알데히드 n-부틸알데히드 i-부틸알데히드 n-발레르알데히드 i-발레르알데히드, 아세트산에틸, 톨로엔, 자일렌, 메틸이소부틸케톤, 이소부탄올에 대해서는 최소감지농도까지 검출할 수 있음을 확인할 수 있었다. 악취성분의 동시 분석 예로서 음식물 쓰레기의 퇴비화 과정에서 발생되는 휘발성 성분을 농축시켜 흡착/열탈착/GC/MSD에 의해 분석하고 각 성분의 농도와 최소 냄새감지 농도로부터 악취원인 성분을 예측하였다. 분석결과 34가지 물질에 대해 확인하였고, 이 중 트리메틸아민, 이소발레르알데히드, 메틸메르캅탄, 메틸알리황, 이메틸황, 아세트알데히드, 에탄올, n-부틸알데히드의 순으로 악위에 기여할 것으로 예상되었다.