• Title/Summary/Keyword: Capillary limit

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Determination of Captan, Folpet, Captafol and Chlorothalonil Residues in Agricultural Commodities using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Captan, Folpet, Captafol 및 Chlorothalonil의 잔류분석법)

  • Lee, Su-Jin;Hwang, Young-Sun;Kim, Young-Hak;Kwon, Chan-Hyeok;Do, Jung-A;Im, Moo-Hyeog;Lee, Young-Deuk;Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
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    • v.29 no.2
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    • pp.165-175
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    • 2010
  • A gas chromatographic (GC) method was developed to determine residues of captan, folpet, captafol, and chlorothalonil, known as broad-spectrum protective fungicides for the official purpose. All the fungicide residues were extracted with acetone containing 3% phosphoric acid from representative samples of five agricultural products which comprised rice, soybean, apple, pepper, and cabbage. The extract was diluted with saline, and dichloromethane partition was followed to recover the fungicides from the aqueous phase. Florisil column chromatography was additionally employed for final cleanup of the extracts. The analytes were then determined by gas chromatography using a DB-1 capillary column with electron capture detection. Reproducibility in quantitation was largely enhanced by minimization of adsorption or thermal degradation of analytes during GLC analysis. Mean recoveries generated from each crop sample fortified at two levels in triplicate ranged from 89.0~113.7%. Relative standard deviations (RSD) were all less than 10%, irrespective sample types and fortification levels. As no interference was found in any samples, limit of quantitation (LOQ) was estimated to be 0.008 mg/kg for the analytes except showing higher sensitivity of 0.002 mg/kg for chlorothalonil. GC/Mass spectrometric method using selected-ion monitoring technique was also provided to confirm the suspected residues. The proposed method was reproducible and sensitive enough to determine the residues of captan, folpet, captafol, and chlorothalonil in agricultural commodities for routine analysis.

Accuracy Evaluation of the Alternative Site Blood Glucose Test Using Error Grid (에러그리드를 사용한 대체부위 혈당검사의 유용성 검증)

  • Park, Kyung-Soon;Cha, Eun-Jong
    • Journal of Biomedical Engineering Research
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    • v.32 no.1
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    • pp.25-31
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    • 2011
  • Blood glucose information is important for self regulation in daily life, but the frequency of self test remains to be only 17%(9 tests/month) in Korea, mainly due to pain during blood sampling. The present study tried to validate the clinical efficacy of the forearm as an alternative sampling site with minimized pain. Capillary blood was sampled both on the index finger($G_F$) and the forearm($G_A$), immediately followed by glucose measurements in 531 subjects, 25 who visited the Health Enhancement Center of C University Hospital, then venous blood($G_V$) was sampled for glucose test. The blood glucose concentration measured on the forearm was closer to the venous glucose than on the finger. The mean difference between $G_V$and $G_F$ was only 10 mg/dL well within the internationally accepted error limit. Error grid analyses of $G_F-G_V$, $G_A-G_V$ and $G_A-G_F$ revealed that the number of data points in regions A and B took 100%, 99.8%, and 97.9%, respectively. These results demonstrate the forearm blood glucose test is not only accurate but also clinically valid. Therefore, the forearm blood glucose test can be a useful way of self managing the chronic diabetes with minimized sampling pain.

Optimization of Gas-Liquid Chromatographic Parameters for the Multiresidue Analysis of 24 Pesticides (잔류농약 24성분의 다성분 동시분석을 위한 기체크로마토그래피 조건의 최적화)

  • Lee, Eun-Ju;Kim, Woo-Seong;Park, Kun-Sang;Oh, Jae-Ho;Kim, Dai-Byung
    • The Korean Journal of Pesticide Science
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    • v.4 no.2
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    • pp.11-17
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    • 2000
  • Optimum parameters were investigated for the simultanious analysis of 24 pesticide residuces using gas-liquid chromatography with electron capture detection. Electronic pressure control(EPC) on column enhanced resolution of 24 analyzes. Using DB-17, SPB-608, and Ultra-2 capillary column without EPC incomplete separation was observed in some pairs of pesticides. When EPC function was adopted, no severe overlapping was observed on SPB-608 column in every pesticides except vinclozolin/acetochlor pair. Total running time was 45 min, much shorter than $69{\sim}81$ min when used without EPC. Limit of determination of each analyze ranged $0.1{\sim}12.9$ ng/mL.

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Chiral Separation of Lactic Acid in Culture Media and Cells of Lactobacillus delbrueckii subsp. lactis as O-Pentafluoropropionylated (S)-(+)-3-Methyl-2-Butyl Ester by Achiral Gas Chromatography-Mass Spectrometry

  • Paik, Man-Jeong;Nguyen, Duc-Toan;Yoon, Jae-Hwan;Chae, Han-Seung;Kim, Kyoung-Rae;Lee, Gwang;Lee, Pyung-Cheon
    • Bulletin of the Korean Chemical Society
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    • v.32 no.7
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    • pp.2418-2422
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    • 2011
  • The enantiomeric separation of lactic acid for its absolute configuration has become important task for understanding its biological origin and metabolic process involved in the formation of lactic acid. It involves the conversion of enantiomers as diastereomeric O-pentafluoropropionylated (S)-(+)-3-methyl-2-butyl ester and the direct separation by gas chromatography-mass spectrometry on a achiral capillary column. The (R)- and (S)-lactic acids were completely separated with a high resolution of 1.9. The newly developed method showed good linearity (r ${\geq}$ 0.999), precision (% relative standard deviation = 3.4-6.2), and accuracy (% relative error = -7.7-1.4) with the detection limit of 0.011 ${\mu}g/mL$. When the method was applied to determine the absolute configuration of lactic acid in Lactobacillus delbrueckii subsp. lactis 304 (LAB 304), the composition (%) of (R)-lactic acid in the cell pellet and in the culture medium were $89.0{\pm}0.1$ and $78.2{\pm}0.4$, respectively. Thus, it was verified that the present method is useful for the identification and composition test of lactic enantiomers in microorganisms.

Studies on the Simultaneous Determination of VNA and TSNA by GC - TEA (Gas chromatography-Thermal Energy Analyzer에 의한 휘발성 니트로소아민과 담배 특유의 니트로소아민들의 동시 분석연구)

  • Rhee, Mun-Su;Ji, Sang-Woon;Park, Yang-Su
    • Journal of the Korean Society of Tobacco Science
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    • v.15 no.2
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    • pp.174-184
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    • 1993
  • This is to investigate the methodology for the simultaneous determination of Wk, mk and TSNA using gas chromatography(GC) in combination with chemiluminescence detector, thermal energy analyzer(TEA) . The simultaneous analysis has been estimated by evaluating tobacco. The TEA was linked to GC equipped with non -polar SPB -5 fused silica capillary column which was introduced into the ceramic pyrolysis tube by the point of 16cm from the end of TEA. Quantification was carried out by internal standardization with WDPA after calibration of retention times and response factors with authentic nitrosoamines. It was demonstrated that WDPA was most preferable as internal standard for the simultaneous analysis. The recoveries of the internal standard were in the range of 83∼96% . Nitrosoamines in this method were detected with determination limit of 0.1ng and was made by a straight line in calibration curve by TEA response. The suitability of nitrosoamines extraction in tobacco leaf was investigated. It was most suitable to extract nitrosoamines from tobacco leaves with 0.01 M NaOH within a period of 8 hours. Thimerosal as an antibacterial agent was added to NaOH solution to prevent artifactual formation. The fractionation and the purification of nitrosoamines form alkaline extracts were conveniently performed using Extrelut multilayer column and dichloromethane. Reproducible and reliable results were obtained for the determination of nitrosamines in a relatively short time compared to previous known method. TSNA contents in burley were about 4 times higher as those in the fluecured tobacco.

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Analytical method of PCDDs/PCDFs in blood using NIST SRM 1589a (인증표준물질(NIST SRM 1589a)을 이용한 혈액 중 다이옥신 분석방법)

  • Shin, Sun Kyoung;Park, Seok Un;Kim, Tae Seung
    • Analytical Science and Technology
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    • v.18 no.6
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    • pp.559-567
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    • 2005
  • For the analytical method of PCDD/Fs in blood, which have been issued recently, SRM 1589a of NIST(National Institute of Standards and Technology) was used and a practical analytical method of PCDD/Fs in blood was presented through comparison of methods of Canada and Japan. The proposed method used alkali-digestion extraction for removal of the lipid effectively using two capillary columns. The limit of quantification of TeCDD/DF and PeCDD/DF was 1 pg/g-lipid, HxCDD/DF and HpCDD/DF was 2 pg/g-lipid, OCDD/DF was 4 pg/g-lipid. With consideration the range of detected concentration, calibration standards were presented as $CS_L$(0.1~1), $CS_1/2$(0.25~2.5), $CS_1$(0.5~5.0), $CS_2$(2~20), $CS_3$(10~100).

Development of species-specific multiplex PCR assays of mitochondrial 12S rRNA and 16S rRNA for the identification of animal species (식육감별을 위한 미토콘드리아 12S rRNA와 16S rRNA 유전자의 종 특이적 multiplex PCR 기법 개발)

  • Koh, Ba-Ra-Da;Kim, Ji-Yeon;Na, Ho-Myung;Park, Seong-Do;Kim, Yong-Hwan
    • Korean Journal of Veterinary Service
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    • v.34 no.4
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    • pp.417-428
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    • 2011
  • Species-specific PCR assay was developed for detection of cattle, sheep, goat, horse, dog, pig, chicken, duck, goose, and turkey using mitochondrial 12S rRNA and 16S rRNA as target genes. Also, an internal positive control was used to detect possible false negatives by using 18S rRNA gene. We designed species-specific primers with amplicon length of 190, 219, 350, 467, 241, 119, 171, 229, 111 and 268 bp for cattle, sheep, goat, horse, dog, pig, chicken, duck, goose, and turkey respectively. The specificity of the primers was tested against the other 10 non-target animal species and a cross-reaction was not observed. We developed two multiplex PCR assays for the simultaneous identification of Korea's major livestock species (cattle, pig, chicken and duck) and poultry species (chicken, duck, goose and turkey) from analogous samples, retaining the same specificity. The limit of detection of the multiplex PCR assay (cattle, pig, chicken and duck) ranged between 1 pg and 0.1 pg of template DNA extracts from raw meat. Applying multiplex PCR assays to DNA extracts from experimental pork/beef and pork/chicken tested raw and heat-treated ($120^{\circ}C$ for 30 min) mixtures respectively, detection limit was 0.1% level beef in pork, pork in beef and chicken in pork and 1.0% level pork in chicken. In conclusion, this assay using gel-based capillary electrophoresis would be very useful in highly sensitive and rapid identification of animal species or ingredients in minced meat and other meat products.

Changes of Salt Concentration by the Height of Ground Water Table on Disused Saltpan for Golf Course Construction Site (골프코스를 조성할 폐염전 매립지의 지하수위에 따른 토양산도 및 전기전도도 변화)

  • Lee, Dong-Ik;Kim, Ki-Dong;Joo, Young-Kyoo
    • Asian Journal of Turfgrass Science
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    • v.23 no.1
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    • pp.143-150
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    • 2009
  • High salt concentration is one of the most important limit factor on plant growth at a disused saltpan for golf course construction site. The control of salt in soil is definitely required and the monitoring of salt concentration in soil and ground water also required to amend soil physiochemical properties. This research was carried out to monitor the pH and salt concentration changes by the height of ground water. By the physiochemical analysis test, the soil contains a high salt concentration and classified as a slight alkaline clay soil. The height of ground water table changed to 1.3m, 3.3m and 2.8m at dry season(mid-late June, 2005), monsoon season(early-mid July) and after monsoon(late July), respectively. Compare to the average ground level of 2.9m, the ground water was over flooded about OAm at monsoon season. The electrical conductivity(ECe) was measured above $4.0dS{\cdot}m^{-1}$ over all areas and however, some areas showed over $20dS{\cdot}m^{-1}$. During a monsoon season, ECe was lowered to $1.2{\sim}15.0dS{\cdot}m^{-1}$, compared with those of the dry season. Therefore, the interception of the capillary connection between planting layer and ground water which contains high salt concentration should be adapted when golf courses are constructed on disused saltpan. The phytotoxicity caused by salt damage may be controled by the interception of capillary fringe of salt flow to the topsoil profile at the upper layer of the ground water table.

Evaluation of Hydrogeologic Seal Capacity of Mudstone in the Yeongil Group, Pohang Basin, Korea: Focusing on Mercury Intrusion Capillary Pressure Analysis (포항분지 영일층군 이암층의 수리지질학적 차폐능 평가: 수은 모세관 압입 시험의 결과 분석을 중심으로)

  • Kim, Seon-Ok;Wang, Sookyun;Lee, Minhee
    • Economic and Environmental Geology
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    • v.53 no.1
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    • pp.23-32
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    • 2020
  • Geological CO2 sequestration is a global warming response technology to limit atmospheric emissions by injecting CO2 captured on a large scale into deep geological formations. The presented results concern mineralogical and hydrogeological investigations (FE-SEM, XRD, XRF, and MICP) of mudstone samples from drilling cores of the Pohang basin, which is the research area for the first demonstration-scale CO2 storage project in Korea. They aim to identify the mineral properties of the mudstone constituting the caprock and to quantitatively evaluate the hydrogeologic sealing capacity that directly affects the stability and reliability of geological CO2 storage. Mineralogical analysis showed that the mudstone samples are mainly composed of quartz, K-feldspar, plagioclase and a small amount of pyrite, calcite, clay minerals, etc. Mercury intrusion capillary pressure analysis also showed that the samples generally had uniform particle configurations and pore distribution and there was no distinct correlation between the estimated porosity and air permeability. The allowable CO2 column heights based on the estimated pore-entry pressures and breakthrough pressures were found to be significantly higher than the thickness of the targeting CO2 injection layer. These results showed that the mudstone layers in the Yeongil group, Pohang basin, Korea have sufficient sealing capacity to suppress the leakage of CO2 injected during the demonstration-scale CO2 storage project. It should be noticed, however, that the applicability of results and analyses in this study is limited by the lack of available samples. For rigorous assessment of the sealing efficiency for geological CO2 storage operations, significant efforts on collection and multi-aspect evaluation for core samples over entire caprock formations should be accompanied.

Simultaneous Pesticide Analysis Method for Bifenox, Ethalfluralin, Metolachlor, Oxyfluorfen, Pretilachlor, Thenylchlor and Trifluralin Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Bifenox, Ethalfluralin, Metolachlor, Oxyfluorfen, Pretilachlor, Thenylchlor 및 Trifluralin의 동시 분석)

  • Ahn, Kyung Geun;Kim, Gi Ppeum;Hwang, Young Sun;Kang, In Kyu;Lee, Young Deuk;Choung, Myoung Gun
    • Korean Journal of Environmental Agriculture
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    • v.37 no.2
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    • pp.104-116
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    • 2018
  • BACKGROUND: This experiment was conducted to establish a simultaneous analysis method for 7 kinds of herbicides in 3 different classes having similar physicochemical property as diphenyl ether(bifenox and oxyfluorfen), dinitroaniline (ethalfluralin and trifluralin), and chloroacetamide (metolachlor, pretilachlor, and thenylchlor) in crops using GC-ECD/MS. METHODS AND RESULTS: All the 7 pesticide residues were extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and directly partitioned into n-hexane/dichloromethane(80/20, v/v) to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. The analytes were separated and quantitated by GLC with ECD using a DB-1 capillary column. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop samples fortified with bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries of the 7 pesticide residues ranged from 75.7 to 114.8% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of the analytes were 0.004 (etahlfluralin and trifluralin), 0.008 (metolachlor and pretilachlor), 0.006 (thenylchlor), 0.002 (oxyfluorfen), and 0.02 (bifenox) mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residues. Therefore, this analytical method was reproducible and sensitive enough to determine the residues of bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin in agricultural commodities.