• Title/Summary/Keyword: GC/MSD

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Detection and Quantitation of Residual Antibiotics and Antibacterial Agents in Foods

  • Ryu, Jae-Chun;Seo, Ja-Won;Song, Yun-Seon;Park, Jong-Sei
    • Journal of Food Hygiene and Safety
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    • v.5 no.3
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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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Analysis of Blood Toluene and Butane in Death Cases of Inhalant Abusers (사망사고 관련된 유해화학 물질 남용자들의 혈액 중 톨루엔과 부탄의 분석)

  • Kim, Nam-Yee;Yang, Young-Geun;Chung, Hee-Sun;Park, Sung-Woo
    • Analytical Science and Technology
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    • v.12 no.6
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    • pp.577-582
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    • 1999
  • The blood toluene concentration was determined by using the GC/MSD with HS-SPME technique in postmortem blood, quantitatively. Butane gases was analyzed by using the GC/FID with HS technique in postmortem blood, qualitatively. Seventy five cases of dead associated with inhalation of glue or butane gases happened in Korea for the last 3 years (1996-1998). In 27 cases of deah due to glue sniffing, nine persons died as a result of a fall while intoxication and their blood tolucne concentration was fairly high in the range of $1.3{\sim}21.6{\mu}g/mL$. In case of death due to butane sniffing, fifty four persons died of acute butane gases inhalation or suffocation, and 6 persons died of butane gases as well as glue inhalation.

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Volatile components of chamomile(Matricaria Chamomilla L.) cultivated in Korea (한국산 카모밀의 향기 성분)

  • Kim, Young-Tae;Park, Joon-Young;Kim, Ok-Chan;Chang, Hee-Jin;Kim, Young-Hoi;Ra, Do-Young
    • Applied Biological Chemistry
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    • v.35 no.2
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    • pp.122-125
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    • 1992
  • The essential oils from whole plant, flower, seed, stem and leaves of domestic chamomile were extracted by simultaneous distillation-extraction and analyzed by GC/ MSD/IRD and retention index matching. The experimental results revealed the presence of over 31 volatile components. Major components were chamazulene, bisabolol, bisabolol oxide A, B. The contents of these major components which possess the pharmacological effects were found to be flower(75.1%), seed(76.6%), stem and leaves(10.09%), whole plant (48.9%), respectively, in domestic chamoile oil, whereas found to be flower(49.2%) in foreign chamomile oil. These results suggest that the usefulness of domestic chamomile is promising because of high contents of these four major components which posses pharmacological effects.

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The Determination of 5-Fluorourasil in Human Plasma by a Gas Chromatography-Mass Spectrometry (GC-MS에 의한 혈중 5-fluorouracil의 정량법)

  • Shin, Ho-Sang;Seo, Bae-Seck;Oh, Yun-Suk;Park, Sung-Woo
    • Analytical Science and Technology
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    • v.11 no.1
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    • pp.36-41
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    • 1998
  • A gas chromatography-mass spectrometry method for the determination of 5-fluorourasil in human plasma is described. The method involves a single extraction procedure with 10 ml of isopropanol-ether(20:80) solution and pentafluoro-benzylation. Samples were injected using an automatic injector, followed by separation on a nonpolar capillary column and detection with a mass selective detector(MSD). No endogeneous compounds were found to interfere. The detection limit, based upon an assayed plasma volume of 0.5, was 3 ng/ml. The extraction yield was found to be above 80%. Plasma 5-FU concentrations were determined by this method in about 500 plasma samples from cancer patients undergoing treatment with 5-FU. This method is suitable for monitoring of 5-FU in plasma of cancer patients.

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

  • Sungjun, Woo;Kwonchul, Ha
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.32 no.4
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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.

Determination of residual pesticides in crude drugs - Gas chromatographic Analysis of 18 pesticides - (한약재중의 잔류농약 분석 - GC에 의한 18종 잔류농약의 분석 -)

  • Hwang, In-Sook;Choi, Byung-Hyun;Bae, Chong-Ho;Kim, Myung-Hee;Cho, Hae-Jeon
    • Korean Journal of Pharmacognosy
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    • v.32 no.3 s.126
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    • pp.200-211
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    • 2001
  • This study was carried out to determine the 11 organochlorine, 7 organophosphorus residual pesticides in 251 crude drugs. These residual pesticides in herbal drugs were extracted with acetonitrile and the extracts were cleaned up via LC-florisil solid phase extraction column. The prepared samples were assayed for pesticide residues using GC-ECD, NPD with capillary column and identified by GC-MSD. Recoveries were $63.9{\sim}111.5%$ in the organochlorine pesticides and $69.8{\sim}92.4%$ in the organophosphorus pesticides, and detection limits were $0.001{\sim}0.65\;ppm$ in the organochlorine pesticides and $0.0009{\sim}0.0074\;ppm$ in the organophosphorus pesticides. Pesticide residues were detected in 9 cases.

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Residual Pesticides in Dried Agricultural Products Collected from Gyeonggi Province (경기도내 유통 건조농산물의 잔류농약 실태)

  • Lee, Myung-Jin;Kim, Myung-Gil;Jeong, Hong-Rae;Yun, Hee-Jeong;Kim, Nan-Young;Kim, Han-Taek;Kim, Chol-Young;Lee, Woon-Hyung;Yoon, Mi-Hye
    • The Korean Journal of Pesticide Science
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    • v.15 no.3
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    • pp.238-245
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    • 2011
  • This study was carried out to examine residual pesticides in dried agricultural products collected from Gyeonggi province in 2010. A total of 102 samples was collected and analyzed for 206 pesticides by multiresidue method using GC-${\mu}ECD$, GC-NPD, GC/TOF/MSD, HPLC-UVD, HPLC-FLD and HPLC/MS/MS. The detection rate of residual pesticides was 23.5% (24 of 102 samples) and the agricultural products exceeding their MRLs (Maximum Residue Limits) were 1 sample of pepper leaves. Additionally, the frequently detected pesticide were chlorothalonil, fenvalerate, chlorpyrifos, endosulfan, bifenthrin, cypermethrin, hexaconazole and iprodione. The pesticide types detected in the dried agricultural products showed in the descending order of organophosphorus (22%), pyrethroid (22%), organochloride (17%), dicarboxymide (11%), carboxymide (6%), carbamate (6%), triazole (5%) and the others (11%).

Monitoring and risk assessment of pesticide in school foodservice products in seoul, Korea (서울지역 학교급식 식재료의 잔류농약 위해성 평가)

  • Seo, Young-Ho;Moon, Kwang-Deog
    • Food Science and Preservation
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    • v.21 no.1
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    • pp.69-74
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    • 2014
  • We tested for residual pesticide levels in school foodservice agricultural products in Seoul, Korea from 2010 to 2012. A total of 316 samples of 23 different types of agricultural products were analyzed via gas chromatography-nitrogen phosphate detector (GC-NPD), an electron capture detector (GC-${\mu}ECD$), a mass spectrometry detector (GC-MSD), and a high performance liquid chromatography-ultraviolet detector (HPLC-UV). We used multi-analysis methods to analyze 185 different pesticide types. Among the selected agricultural products, residual pesticides were detected in 26 samples (8.2%), of which 6 samples (1.9%) exceeded the Korea Maximum Residue limits (MRLs). We detected pesticide residue in more than 65% of the Chwinamul, while 6 among 9 analyzed samples contained pesticide residue, and 1 sample exceeded the Korea MRLs. Among the 185 kinds of pesticides that we have tested, 18 were detected, while 7 of them were detected more than twice. Data obtained were then used for estimating the potential health risks associated with the exposures to these pesticides. The most critical commodity is carbofuran in the perilla leaves, which has contributed 3.8% to the hazard index (HI). These results showed that the detected pesticides could not be considered as a serious public health problem. Nevertheless, constant supervision is recommended.

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

  • Sung, Ki-Chun
    • Journal of the Korean Applied Science and Technology
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    • v.29 no.3
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    • pp.402-411
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    • 2012
  • Natural Bokbunja is used as a material of oriental medicine which it obtains from Rubus or Raspberry. Natural Bokbunja Rubus has natural odor and taste, natural color, and pharmaceutical & chemical characteristics. This experiment tested antimicrobial experiment against microbe and dye experiment against fiber using natural Bokbunja extract. Some conclusions from this characteristics experiment were obtained as follow. The result of antimicrobial experiment could know that ATCC-001(staphylococcus aureus) does not show nearly from 72hrs after cultivation test and ATCC-002(aspergillus niger) shows to propagate continuously according to passage of time. Also, the result of dye experiment could know that cotton and silk using alum mordant($Al_2(SO_4)_3{\cdot}13-14H_2O$) against fiber shows in direction of light beige color. The result of instrument analysis ascertained inorganic components of K(221.100ppm), Mg(17.920ppm), Ca(5.129ppm), Na(2.940ppm), Si(0.638ppm) etc from Bokbunja with ICP/OES, and ascertained organic components of boric acic(1.711), silane(2.142), pyrazole(3.481), propyl isothiocyanate(2.565), furfurole(11.521) etc from Bokbunja with GC/MSD.

Studies on the Quantitative analysis and the Health Effect of VOCs in Environment - Analysis for THMs of tap water in six cities of Korea - (VOCs 측정 및 VOCs가 인체에 미치는 영향에 관한 연구 - 우리나라 6개 대도시 수도수 중 THMs 분석 -)

  • Kim, Mi-Kyoung;Park, Yuon-Sin;Chung, Yong
    • Analytical Science and Technology
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    • v.13 no.1
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    • pp.55-65
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    • 2000
  • In this study, we collected the tap water that treated from water plant in Seoul, Incheon, Taejon, Kwangju, Taeku and Pusan and supplied each house. The sampling period was June and September, 1997. The concentration of THMs formed by chlorination in drinking water was determined with the purge and trap method with GC/MSD recommended by the us EPA 542.2 method. Chloroform is the most of THMs (47.43%~93.11%) and the content order is bromodichloromethane > chlorodibromomethane > bromoform. In Incheon, Taejon, Kwangju, Taeku and Pusan, the content of bromodichloromethane, chlorodibromomethane and bromoform was higher than Seoul. But, in June and September, the concentration of THMs in six cities is not over Korea Drinking Water Regulation $100{\mu}g/L$. The calculated human exposure for each substances were chloroform $6.14{\times}10^{-4}mg/kg/day$, bromodichloromethane $1.01{\times}10^{-4}mg/kg/day$, chlorodibromomethane $0.29{\times}10^{-4}mg/kg/day$, bromoform $0.01{\times}10^{-4}mg/kg/day$ and THMs $7.98{\times}10^{-4}mg/kg/day$.

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