• Title/Summary/Keyword: packed column

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Evaluation of Organochlorine Pesticide Residues in the Mud Flat (연안(沿岸) 패류(貝類) 서식지(棲息地) 저니토중(底泥土中) 유기염소계(有機鹽素系) 농약(農藥)의 잔류평가(殘留評價))

  • Suh, Yong-Tack;Im, Geon-Jae;Shim, Jae-Han
    • Korean Journal of Environmental Agriculture
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    • v.5 no.2
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    • pp.113-118
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    • 1986
  • After selecting four places in the main shellfish habitat, 118 items of the sample were collected in the mud flat from August to October in 1983, in order to analyze organochlorine pesticide residues by a gas chromatograph equipped with an electron capture detector. The results obtained were summarized as follows; ${\alpha}-BHC,\;{\gamma}-BHC\;&\;PCNB,\;heptachlor,\;{\gamma}-endosulfan,\;{\beta}-endosulfan,$ p, p'-DDE, dieldrin, o, p'-DDT and p, p'-DDT were detected in the range from 2 to 98 percent and their levels of mean residues ranged from trace to 0.041ppm, in the order of ${\gamma}-BHC\;&\;PCNB,\;{\alpha}-BHC,\;heptachlor{\approx}{\alpha}-endosulfan{\approx}p, p`-DDE{\approx}dieldrin{\approx}{\beta}-endosulfan{\approx}$o, p'-DDT, and p, p'-DDT. The mean of total residues in regions was Kangjin(0.058ppm), Kwangyang(0.080ppm), Yoch'on (0.016ppm), and Yonggwang(0.75ppm). ${\gamma}-BHC\;&\;PCNB$ peak were separated by column packed with DC-200. PCNB was identified by making a PCA(pentachloroaniline), the reduced derivative of PCNB, and this confirmed that PCNB residues were detected in the soil sample.

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The Effect of Filter Media on the Biofiltration of Air Contaminated by Toluene (톨루엔으로 오염된 공기의 생물학적 여과에 대한 필터용 담체의 영향)

  • 홍성도;한희동;명성운;최호석;김인호
    • KSBB Journal
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    • v.16 no.6
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    • pp.603-608
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    • 2001
  • In this study, we studied on the remeval of toluene vapors in a lab-scale biofilter. Biofiltration was performed in a column fed downflow with contaminated air at ambient conditions. The column was packed with mixture of Peat and Calstene(5:3 vol. Ratio), Synthesized media, Bark and Wood chip, which were inoculated with microbial population of selected stains(Pseudomonas. putida, KCCM 11343, ATCC 12633). The microorganisms were immobilized on the bed medium and then biofilm were formed. The biofilter was operated under the conditions of various inlet toluene concentrations for 180 days and treated up to the elimination capacity of maximum 40 g/㎥hr at the inlet load of 30 g/㎥ hr with percentage removals of 20∼90% and gas retention times between 1 and 2 min. The pressure drop was very negligible through the biofilter columps because its value of 0.054 cmH$_2$O/m was much less than others. The effect of operating conditions such as flow rate, inlet toluene concentration and moisture contents on the performance of the biofilter was sequentially investigated in this study.

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Development of Simultaneous Analysis for the Multi-residual Pesticides in the Ginseng Extract using Gas Chromatography (인삼농축액에서 GC를 이용한 잔류농약 동시다성분 분석법의 개발)

  • Shin Yeong-Min;Lee Seon-Hwa;Son Yeong-Uk;Jeong Ji-Yoon;Jeoung Seoung-Wook;Park Heung-Jai;Kim Sung-Hun;Won Young-Jun;Lee Chang-Hee;Kim Woo-Seong;Hong Moo-Ki;Chae Kab-Ryong
    • Journal of Environmental Science International
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    • v.15 no.1
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    • pp.85-94
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    • 2006
  • The simultaneous analysis of multi-residual pesticides was developed using a gas chromatography (GC) method. In this study, a simple and reliable methodology was improved to detect 154 kinds of pesticides in sinseng extract sample by using a liquid-liquid extraction procedure, open column chromagraphy and chromatographic analysis by CC electron capture detector (ECD) and GC nitrogen-phosphorus detector (NPD). The 154 kinds of pesticides were classified in 4 groups according to the chemical structure. The extraction of pesticides was experimented with $70\%$ acetone and dichloromethane/petroleum ether in order, and cleaned up via open column chromatography $(3\times30cm)$ packed with florisil $(30g,\;130^{\circ}C,\;12hrs)$. The final extract was concentrated in a rotator evaporator at $40^{\circ}C$ until dryness. Then the residue was redissolved to 2ml with acetone, and analyzed by GC-ECD and GC-NPD. The applied concentration of pesticides was over $1\~10{\mu}g/ml$. The recovery tests were ranged from $70.7\%$ to $115.2\%$ with standard deviations between 0.3 and $5.7\%$ of the standard spiked to the ginseng extract sample (Group $I\~IV$). The limit of detection (LOD) ranged from 0.001 to $0.099{\mu}g/ml$ (Group $I\~IV$). The 9 kinds of pesticides were not detected. The developed method was applied satisfactory to the determination of the 154 kinds of pesticides in the ginseng extract with good reproducibility and accuracy.

Full validation of high-throughput bioanalytical method for the new drug in plasma by LC-MS/MS and its applicability to toxicokinetic analysis

  • Han, Sang-Beom
    • Proceedings of the Korean Society of Toxicology Conference
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    • 2006.11a
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    • pp.65-74
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    • 2006
  • Modem drug discovery requires rapid pharmacokinetic evaluation of chemically diverse compounds for early candidate selection. This demands the development of analytical methods that offer high-throughput of samples. Naturally, liquid chromatography / tandem mass spectrometry (LC-MS/MS) is choice of the analytical method because of its superior sensitivity and selectivity. As a result of the short analysis time(typically 3-5min) by LC-MS/MS, sample preparation has become the rate- determining step in the whole analytical cycle. Consequently tremendous efforts are being made to speed up and automate this step. In a typical automated 96-well SPE(solid-phase extraction) procedure, plasma samples are transferred to the 96-well SPE plate, internal standard and aqueous buffer solutions are added and then vacuum is applied using the robotic liquid handling system. It takes only 20-90 min to process 96 samples by automated SPE and the analyst is physically occupied for only approximately 10 min. Recently, the ultra-high flow rate liquid chromatography (turbulent-flow chromatography)has sparked a huge interest for rapid and direct quantitation of drugs in plasma. There is no sample preparation except for sample aliquotting, internal standard addition and centrifugation. This type of analysis is achieved by using a small diameter column with a large particle size(30-5O ${\mu}$m) and a high flow rate, typically between 3-5 ml/min. Silica-based monolithic HPLC columns contain a novel chromatographic support in which the traditional particulate packing has been replaced with a single, continuous network (monolith) of pcrous silica. The main advantage of such a network is decreased backpressure due to macropores (2 ${\mu}$m) throughout the network. This allows high flow rates, and hence fast analyses that are unattainable with traditional particulate columns. The reduction of particle diameter in HPLC results in increased column efficiency. use of small particles (<2 urn), however, requires p.essu.es beyond the traditional 6,000 psi of conventional pumping devices. Instrumental development in recent years has resulted in pumping devices capable of handling the requirements of columns packed with small particles. The staggered parallel HPLC system consists of four fully independent binary HPLC pumps, a modified auto sampler, and a series of switching and selector valves all controlled by a single computer program. The system improves sample throughput without sacrificing chromatographic separation or data quality. Sample throughput can be increased nearly four-fold without requiring significant changes in current analytical procedures. The process of Bioanalytical Method Validation is required by the FDA to assess and verify the performance of a chronlatographic method prior to its application in sample analysis. The validation should address the selectivity, linearity, accuracy, precision and stability of the method. This presentation will provide all overview of the work required to accomplish a full validation and show how a chromatographic method is suitable for toxirokinetic sample analysis. A liquid chromatography/tandem mass spectrometry (LC-MS/MS) method developed to quantitate drug levels in dog plasma will be used as an example of tile process.

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Effect of Biofilter Made of Composted Pine Tree Bark and Perils on Reducing Odor from Pig House (부숙수피-펄라이트 혼합충전재의 돈사악취 제거 효과)

  • Lee, Seung-Joo;Chang, Dong-Il;Chang, Hong-Hee
    • Korean Journal of Environmental Agriculture
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    • v.25 no.2
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    • pp.118-123
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    • 2006
  • To remove effectively order component ($NH_3\;and\;H_2S$) from pig house, biofilter was made of composted pine tree bark and polite and odor removal efficiency was evaluated in the lab and pilot scales. The columns were designed with ${\Phi}120mm{\times}450mm$ (H) and ${\Phi}850mm{\times}900mm$ (H) in the size in the lab and pilot scale testes, respectively. Single material of composted pine tree bark and polite and the mixture of two materials with 7:3 ratios (vol/vol) were packed in the column, and, herein air flow was controlled upward direction from column bottom. To enhance the efficiency of biofilter, ammonia (Rhodococcus equi A3) and hydrogen sulfide oxidizing bacteria (Alcaligenes sp. S5-5.2) were inoculated in packing materials before the test Removal effect of ammonia and hydrogen sulfide gases were higher in the mixture$[88.7{\sim}98.2%,\;89.5{\sim}97.9%]$ than that in single packing material (composted pine tree haft$[89.4{\sim}98.7%,\;78.7{\sim}85.6%]$ and petite$[65.3{\sim}73.2%,\;88.7{\sim}98.2%]$ by the lab scale biofilter. In the modeled pig house, about 96 and 91% of ammonia and hydrogen sulfide gases were removed by the pilot scale of biofilter, respectively. Conclusively, composted pine tree bark and polite could be a good candidate of biofilter packing materials to remove the odor components.

A Study on Quick Quantitative Analyzing Method of Sorbic and Benzoic Acids in Doenjang by Gas Chromatography (기체크로마토그래피에 의한 시판 된장중의 소르빈산과 안식향산의 신속정량법 연구)

  • Park, Kwang-Ja;Lee, Si-Kyung;Kim, Nam-Dae;Cho, Nam-Ji
    • Korean Journal of Food Science and Technology
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    • v.31 no.2
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    • pp.285-292
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    • 1999
  • An analytical method applicable to quality control and its optimum conditions were studied for rapid and efficient analysis of sorbic and benzoic acids used as preservatives in the commercial soybean paste. In gas chromatographic analysis of sorbic and benzoic acids, the application of HP-FFAP (acid modified polyethylene) wide bore column improved the separation ability significantly. By setting the oven temperature of GC to $200^{\circ}C$, the total elapsed time for quantitative analysis was also reduced to the level required in using packed column. By extracting sorbic and benzoic acids from soybean paste with an automatic steam distillation device, the elapsed time for analysis was reduced by 80% more compared to using conventional steam distillation method. The recoveries of sorbic and benzoic acids by the automatic steam distillation were 98.1% and 99.9%, respectively. The sorbic acid was found in 3 samples of 14 commercial soybean pastes, of which contents were $466{\sim}530ppm$, while $0.3{\sim}4.4ppm$ of benzoic acid was found in all the samples.

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Isolation of Alliin in Garlic and Its Quantitative Determination by High Performance Liquid Chromatography and Studies on the Antimicrobial Efforts of Alliin and Ethanol Extracts from Korean Garlic(Alliium sativum L.) (마늘 중 고속 액체 크로마토그래피에 의한 알린의 분리 및 정량과 Alliin과 에탄올 추출물의 항균효과에 관한 연구)

  • 위성언
    • The Korean Journal of Food And Nutrition
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    • v.16 no.4
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    • pp.296-302
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    • 2003
  • First. the purification and analysis of alliin in garlic from different origins by alliin-HPLC determination method were studied. Allinase in garlic was inactivated by heating in boiling water followed by extraction of alliin in garlic with 80% methanol. To remove free amino acids and alliin homologs in garlic, garlic extract was separated by cation exchange column which was packed with amberlite CG-120 resin using 40L d-water as eluent. Alliin in garlic extract was crystallized in a mixture of acetone (50$^{\circ}C$):H$_2$O:acetic acid=70:29:1 and then recrystallized in a mixture of acetone (50$^{\circ}C$):H$_2$O:acetic acid=75:24:1. Obtained alliin was identified by melting point. TLC, microscope observation and mass spectrometry. High performance liquid chromatography (HPLC) following pre-column derivatization of cystein derivatives with o-phthaldialdehyde/2-mercaptoethanol has succeessfully been applied to the analysis of various garlics. Each alliic of standard solution and garlic extract was derivatized to isoindole derivative by o-phthaldialdehyde /2-mercaptoethanol and then analyzed by HPLC. Six point calibration was done by using alliin peak area. Lineality was observed at 0 ∼ 1.0mg/ml of alliin concentration. Weighted regression line function was Y=6254X - 256077. By this function, alliin contents in various garlics were 0.34 ∼ 0.73% fresh weight. Second study was designed to evaluate the effects of garlic extracts of various concentrations on the growth of various pathogenes (Eubacterium limonsum, Bacteroides fragilis, Salmonella typhimurium, Salmonella typhi, Shigella sonnei, Kiebsiella pneumoniae, Enterobacter cloacae, Pserdomonas aeruginosa, Escherichia coli). For antimicrobial effects against microorganism, totally minimal inhibition concentrations (MIC) of alliin were from 5,000 to 20,000ppm. MIC of ethanol extract were 1,250 to 10,000ppm.

A Rapid Method for Determination of ATP and Its Related Compounds in Dried Fish and Shellfish Products Using HPLC (HPLC에 의한 시판수산건제품의 ATP분해생성물의 신속정량법)

  • LEE Eung-Ho;KOO Jae-Geun;AHN Chang-Bum;CHA Yong-Jun;OH Kwang-Soo
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.17 no.5
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    • pp.368-372
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    • 1984
  • This paper deals with a rapid method for determination of ATP and its related compounds in fish and shellfish products using high performance liquid chromatography(HPLC). The HPLC used is a HPLC/ALC-224 equiped with UV-spectrophotometer (254 nm) as detector and integrator (Yanagimoto system-1000). The column used is a stainless steel tubing ($30.0\;cm{\times}3.9\;mm\;i.d.$) packed with ${\mu}-Bon-dapak\;C_{18}$. A mixture of $1\%$ triethylamine-phosphoric acid(pH6.5) was used as an eluent and the flow rate of the eluent was controlled at 2 ml/min. For the separation of ATP and its related compounds, a standard mixture of ATP, ADP, AMP, IMP, inosine and hypoxanthine was subjected to HPLC under the above mentioned conditions. Six peaks were obtained with retention times within 20 min, and elution order were hypoxanthine, IMP, inosine, AMP, ADP and ATP. But 5'-IMP and 5'-GMP fractions were not separated by this method. In generally, IMP content in boiled-dried fish and shellfish products purchased from the market was comparatively higher than that of other nucleotides. Especially, boiled-dried big eye herring marked higher value in IMP content than other boiled-dried ones. Hypoxanthine and inosine were major components of ATP-related compounds in dried products and seasoned-dried ones. And IMP content in seasoned-dried products was higher than that of dried ones. This fact is suggested that a part of IMP in seasoned-dried ones was derived from flavoring matter (MSG, 5'-IMP and 5'-GMP) which is added during the seasoning treatment.

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Cation Exchange Separation and Determination of Ruthenium in a Simulated Spent Nuclear Fuel (모의 사용후핵연료에 함유된 루테늄의 양이온교환 분리 및 정량)

  • Suh, Moo-Yul;Sohn, Se-Chul;Lee, Chang-Heon;Choi, Kwang-Soon;Kim, Do-Yang;Park, Yeong-Jae;Park, Kyoung-Kyun;Jee, Kwang-Yong;Kim, Won-Ho
    • Journal of the Korean Chemical Society
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    • v.44 no.6
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    • pp.526-532
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    • 2000
  • Cation exchange separation and inductively coupled plasma atomic emission spectrometric(ICP-AES) determination of ruthenium in HCl solutions were studied to quantitatively determine ruthenium in spent nuclear fuels. Ruthenium-bearing samples were dissolved with the mixed acid solution(9 : 1 mole ratio, HCl-HNO$_3$) using an acid digestion bomb. Based on the absorption spectra and ion exchange behaviour of ruthenium in hydrochloric acid media, its possible chemical species were discussed. On a cation exchange column (0.7 ${\times}$ 8.0 cm) packed with AG 50W ${\times}$ 8(100~200 mesh) and equilibrated with 0.5 M HCl, ruthenium was eluated with 0.5 M HCl while uranium was retained on the column. The established separation method was applied to a simulated spent nuclear fuel and resulted in the recovery of 98.5% with a relative standard deviation of 0.7%.

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Research Possibility of Using Quartz Crystal Microbalance for Polystyrene Nanoplastics Adsorption to SiO2 Surface (수정진동자미세저울을 활용한 폴리스티렌 나노플라스틱의 SiO2 표면흡착 연구 가능성)

  • Myeong, Hyeonah;Kim, Juhyeok;Lee, Jin-Yong;Kwon, Kideok D.
    • Korean Journal of Mineralogy and Petrology
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    • v.34 no.4
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    • pp.265-275
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    • 2021
  • Findings of microplastics and nanoplastics from diverse natural environments have increased demand for research of the fate and transport of the potentially toxic plastic particles in soils and groundwater. Weathering of microplastics would generate a significant amount of nanoplastics, but nanoplastics research is scarce because of technical difficulties in detecting nanoplastics in environments and analyzing nanoplastics adsorption to mineral surfaces. In the current study, we tested a possibility using quartz crystal microbalance (QCM) for application to nanoplastics adsorption analysis on mineral surfaces. In silica (SiO2)-packed column experiments, a measurable adsorption capacity for polystyrene nanoparticles often requires injection of unrealistically high ionic strengths or concentrated nanoplastic particles. The current test shows that QCM can measure polystyrene nanoplastics adsorbed onto SiO2 surface under the low ionic strengths and nanoplastics concentrations, where typical column experiments cannot. QCM is a promising tool for understanding the interaction between nanoplastics and mineral surfaces and thus transport of nanoplastics in soils and groundwater.