• Title/Summary/Keyword: GC-determination

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Analytical Determination of Alkylphenols, Chlorophenols and Bisphenol A in Biota Samples using Gas Chromatography/Mass Spectrometry (기체 크로마토그래피/질량분석기를 이용한 생물시료 중 알킬 페놀류, 클로로페놀류 및 비스페놀 A의 분석법)

  • Hong, Jongki;Kim, Hyup;Baek, In-Girl;Kim, Do-Gyun;Seo, Jung-Joo;Seo, Jong-Bok;Chung, Bong-Chul;Pyo, Hee-Soo;Kim, Kyung-Rae;Kim, Yong-Hwa
    • Analytical Science and Technology
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    • v.13 no.4
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    • pp.484-493
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    • 2000
  • The simultaneous analysis of alkylphenols, chlorophenols and bisphenol A in biota samples was performed by gas chromatography-mass spectrometry-selected ion monitoring mode. The phenols were extracted from sample with organic solvent and Forisil and Silica columns for clean-up procedure were compared. Recovery studies were performed at 1-ppm level of phenols added to each biota sample. Their recoveries ranged between 83 and 116% with coefficient of variations of 2.4-11.9%. To improve the detection limits of phenols, trimethylsilyl (TMS) derivatization was applied. The gas chromatographic properties of free phenols and TMS derivatized phenols were also investigated.

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Effect of Arrowroot Flower (Puerariae flos) Extract on Lowering of Ethanol Concentration in Rat Blood (갈화(Puerariae flos)추출물이 Rat 혈중 Ethanol 농도에 미치는 영향)

  • Kim, Jeong-Han;Min, Sun-Sik;Kim, Sung-Hoon;Hong, Heu-Do;Kim, Jong-Soo;Kim, Soo-Un
    • Applied Biological Chemistry
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    • v.38 no.6
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    • pp.549-553
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    • 1995
  • Ethanol concentration in blood, brain and liver of rats was shown to be effectively lowered by arrowroot flower extract. The lowering effect for ethanol concentration in blood was maximum when measured after 1 hour from ethanol feeding. Hot water extract was more effective than 80% ethanol extract. The treatment of extract at 10 min. before ethanol feeding gave a better result than that at 10 min after or 1 hour before ethanol feeding. The ethanol concentration in brain and liver was lowered as found in the blood ethanol concentration. Acetaldehyde was not detected either in blood or the tissues. The optimal amount of the Puerariae flos was 55.7 mg/kg body weight. The newly developed analytical method using dichloromethane as extracting solvent was proven to be very effective in terms of speed and simplicity.

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Determination of Trichlorfon Pesticide Residues in Milk via Gas Chromatography with μ-Electron Capture Detection and GC-MS

  • Hem, Lina;Khay, Sathya;Choi, Jeong-Heui;Morgan, E.D.;El-Aty, A.M. Abd;Shim, Jae-Han
    • Toxicological Research
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    • v.26 no.2
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    • pp.149-155
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    • 2010
  • The pesticide trichlorfon is readily degraded under experimental conditions to dichlorvos. A method has therefore been developed by which residues of trichlorfon in milk are determined as dichlorvos, using gas chromatography with ${\mu}$-electron capture detection. The identification of dichlorvos was confirmed by mass spectrometry. Milk was extracted with acetonitrile followed by centrifugation, freezing lipid filtration, and partitioning into dichloromethane. The residue after partitioning of dichloromethane was dissolved in ethyl acetate for gas chromatography. Recovery concentration was determined at 0.5, 1.0, and 2.0 of times the maximum permitted residue limits (MRLs) for trichlorfon in milk. The average recoveries (n = 6) ranged from 92.4 to 103.6%. The repeatability of the measurements was expressed as relative standard deviations (RSDs) ranging from 3.6%, to 6.7%. Limit of detection (LOD) and limit of quantification (LOQ) were 3.7 and $11.1{\mu}g/l$, respectively. The accuracy and precision (expressed as RSD) were estimated at concentrations from 25 to $250{\mu}g/l$. The intra- and inter-day accuracy (n = 6) ranged from 89.2% to 91% and 91.3% to 96.3%, respectively. The intra- and inter-day precisions were lower than 8%. The developed method was applied to determine trichlorfon in real samples collected from the seven major cities in the Republic of Korea. No residual trichlorfon was detected in any samples.

Determination of Electron Beam-Irradiation by the Chemical Detection Methods According to Storage Period in Fat-riched Agricultural Products (화학적 특성검지에 의한 지방산 고함유 농산물의 저장기간에 따른 전자선 조사 여부 검지)

  • Kim, Dong Yong;Baek, Ji Yeong;Ryu, Hyung Won;Jin, Chang Hyun;Choi, Dae Seong;Yook, Hong-Sun;Byun, Myung-Woo;Jeong, Il Yun
    • Journal of Radiation Industry
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    • v.5 no.4
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    • pp.297-303
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    • 2011
  • The purpose of this research is to detect whether agricultural products were electron beam irradiated or non-irradiated by chemical methods according to increase of storage period. The three fat-rich samples including soybean, walnut, and sesame were chosen as agricultural products, and then were irradiated with doses of 1~10 kGy by using 10 MeV electron beam facility. At the result, 8-heptadecene and 1,7-hexadecadiene, which are indicators of electron beam-irradiation in chemical methods by gas chromatography/mass spectrometry(GC/MS) method, were detected in all three samples. The levels of two irradiation indicators were increased by electron beam-irradiation in a dose-dependent manner. Furthermore, two irradiation indicators also were detected in all samples in 6 and 12 months after irradiation, though levels of those were decreased in a time-dependent manner. These results mean that the quantification of 8-heptadecene and 1,7-hexadecadiene could determine whether electron beam were irradiated or non-irradiated until 12 month after irradiation in 3 fat-rich agricultural products including soybean, walnut, and sesame.

Assessment on the Extraction Efficiency of Explosive Compounds in Soil for Improving the Working Draft of International Standard (국제표준(안) 개선을 위한 토양 중 화약물질 추출 효율성 평가)

  • Lee, Goon-Taek;Jung, In-Ho;Kim, Bo-Hyun;Kim, Dong-Wook
    • Journal of Soil and Groundwater Environment
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    • v.17 no.1
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    • pp.42-46
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    • 2012
  • The ISO document of ISO/TC/190/SC3/WG11/N11 is a working draft of international standard (WD) dealing with analytical method for the determination of explosives and related compounds using high performance liquid chromatography. The scope of this WD covers the storage of samples, preparing test portion, extraction and instrumentation. The main purpose of this study was to improve the extraction conditions which were already adopted in the WD. For this purpose, mechanical shaking method could be corresponded up to 18 hours of ultrasonic bath extraction in the WD was tested. Methanol was also tested with the intention of being added as an extracting solvent other than acetonitrile in the WD. According to the results, 16 hours of mechanical shaking method showed statistically the same effectiveness as that of 18 hours of ultrasonic bath extraction. In case of extracting solvent, methanol also showed statistically the same extraction capability as acetonitrile for DNB, TNT, 2-A-DNT and 2,4-DNT. However, the recovery rate of TNB with methanol extraction was 40% higher than that of acetonitrile extraction. Through adding mechanical shaking method into committee draft (cf. the next stage draft of the WD during the process for making international standard), ISO standard of analyzing explosives and related compounds in soil would become more useful in dealing with huge number of field samples in the laboratory. In other aspect, adopting methanol as an alternative extracting solvent would be very effective in the terms of exchangeability with GC-ECD/MS method which is being developed by German experts.

In vivo wear determination of novel CAD/CAM ceramic crowns by using 3D alignment

  • Aladag, Akin;Oguz, Didem;Comlekoglu, Muharrem Erhan;Akan, Ender
    • The Journal of Advanced Prosthodontics
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    • v.11 no.2
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    • pp.120-127
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    • 2019
  • PURPOSE. To determine wear amount of single molar crowns, made from four different restoratives, and opposing natural teeth through computerized fabrication techniques using 3D image alignment. MATERIALS AND METHODS. A total of 24 single crowns (N = 24 patients, age range: 18 - 50) were made from lithium disilicate (IPS E-max CAD), lithium silicate and zirconia based (Vita Suprinity CAD), resin matrix ceramic material (Cerasmart, GC), and dual matrix (Vita Enamic CAD) blocks. After digital impressions (Cerec 3D Bluecam, DentsplySirona), the crowns were designed and manufactured (Cerec 3, DentsplySirona). A dualcuring resin cement was used for cementation (Variolink Esthetic DC, Ivoclar). Then, measurement and recording of crowns and the opposing enamel surfaces with the intraoral scanner were made as well as at the third and sixth month follow-ups. All measurements were superimposed with a software (David-Laserscanner, V3.10.4). Volume loss due to wear was calculated from baseline to follow-up periods with Siemens Unigraphics NX 10 software. Statistical analysis was accomplished by Repeated Measures for ANOVA (SPSS 21) at = .05 significance level. RESULTS. After 6 months, insignificant differences of the glass matrix and resin matrix materials for restoration/enamel wear were observed (P>.05). While there were no significant differences between the glass matrix groups (P>.05), significant differences between the resin matrix group materials (P<.05) were obtained. Although Cerasmart and Enamic were both resin matrix based, they exhibited different wear characteristics. CONCLUSION. Glass matrix materials showed less wear both on their own and opposing enamel surfaces than resin matrix ceramic materials.

Simultaneous estimation of fatty acids contents from soybean seeds using fourier transform infrared spectroscopy and gas chromatography by multivariate analysis (적외선 분광스펙트럼 및 기체크로마토그라피 분석 데이터의 다변량 통계분석을 이용한 대두 종자 지방산 함량예측)

  • Ahn, Myung Suk;Ji, Eun Yee;Song, Seung Yeob;Ahn, Joon Woo;Jeong, Won Joong;Min, Sung Ran;Kim, Suk Weon
    • Journal of Plant Biotechnology
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    • v.42 no.1
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    • pp.60-70
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    • 2015
  • The aim of this study was to investigate whether fourier transform infrared (FT-IR) spectroscopy can be applied to simultaneous determination of fatty acids contents in different soybean cultivars. Total 153 lines of soybean (Glycine max Merrill) were examined by FT-IR spectroscopy. Quantification of fatty acids from the soybean lines was confirmed by quantitative gas chromatography (GC) analysis. The quantitative spectral variation among different soybean lines was observed in the amide bond region ($1,700{\sim}1,500cm^{-1}$), phosphodiester groups ($1,500{\sim}1,300cm^{-1}$) and sugar region ($1,200{\sim}1,000cm^{-1}$) of FT-IR spectra. The quantitative prediction modeling of 5 individual fatty acids contents (palmitic acid, stearic acid, oleic acid, linoleic acid, linolenic acid) from soybean lines were established using partial least square regression algorithm from FT-IR spectra. In cross validation, there were high correlations ($R^2{\geq}0.97$) between predicted content of 5 individual fatty acids by PLS regression modeling from FT-IR spectra and measured content by GC. In external validation, palmitic acid ($R^2=0.8002$), oleic acid ($R^2=0.8909$) and linoleic acid ($R^2=0.815$) were predicted with good accuracy, while prediction for stearic acid ($R^2=0.4598$), linolenic acid ($R^2=0.6868$) had relatively lower accuracy. These results clearly show that FT-IR spectra combined with multivariate analysis can be used to accurately predict fatty acids contents in soybean lines. Therefore, we suggest that the PLS prediction system for fatty acid contents using FT-IR analysis could be applied as a rapid and high throughput screening tool for the breeding for modified Fatty acid composition in soybean and contribute to accelerating the conventional breeding.

The analysis of ethylene glycol and metabolites in biological specimens (생체시료에서 에틸렌 글리콜과 그 대사체 분석에 관한 연구)

  • Park, Seh-Youn;Kim, Yu-Na;Kim, Nam-Yee
    • Analytical Science and Technology
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    • v.24 no.2
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    • pp.69-77
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    • 2011
  • Ethylene glycol (EG) is produced commercially in large amounts and is widely used as antifreeze or deicing solution for cars, boats, and aircraft. EG poisoning occurs in suicide attempts and infrequently, either intentionally through misuse or accidental as EG has a sweet taste. EG has in itself a low toxicity, but is in vivo broken down to higher toxic organic acids which are responsible for extensive cellular damage in various tissues caused principally by the metabolites glycolic acid and oxalic acid. The most conclusive analytical method of diagnosing EG poisoning is determination of EG concentration. However, victims are sometimes admitted at a late stage to hospitals or died during emergency treatment like a gastric lavage or found rotten dead, when blood EG concentrations are low or not detected. Therefore, in this study, the identification of EG was not only performed by gas chromatograpyc-mass spectrometry (GC-MS) following derivatization but also further toxicological analyses of metabolites, glycolic acid (GA) and oxalic acid (OA), were performed by ion chromatography in various biological specimens. A ranges of blood concentrations (3 cases) was $10\sim2,400\;{\mu}g/mL$ for EG, $224\sim1,164\;{\mu}g/mL$ for GA and ND $\sim40\;{\mu}g/mL$ for OA, respectively, In other biological specimens (liver, kidney, bile and pleural fluid), a range of concentrations (3 cases) was ND $\sim55,000\;{\mu}g/mL$ for EG, ND $\sim1,124\;{\mu}g/mL$ for GA and ND $\sim60\;{\mu}g/mL$ for OA, respectively. Liver and kidney tissues were recommended specimens including blood because OA, a final metabolite of EG, was identified large amounts in these despite no detectable EG caused by some therapy.

Determination of Hydrolysis Rate Constants on Phosphamidon and Profenofos (Phosphamidon과 Profenofos의 가수분해속도 상수의 측정)

  • Min, Kyung-Jin;Ha, Young-Duck;Seo, Seol;Cha, Chun-Geun;Park, Jang-Woo;Lee, Seung-Gon
    • Journal of Food Hygiene and Safety
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    • v.15 no.2
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    • pp.144-150
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    • 2000
  • The present study was peformed to determine the hydrolysis rate constants and degradation products of phosphamidon and proffnofos by the OECD method. Hydrolysis rate constants of phosphamidon in pH 4, pH 7, and pH 9 buffer solutions at 25 and 40$^{\circ}$C were 0.0020, 0.0022, 0.0049 and 0.0040, 0.0050, 0.0150, respectively. Hydrolysis rate of phosphamidon was accelerated by temprerature change under same pH conditions, and half-life of phosphamidon in pH 9 at 40。C was 3 times faster than that at 25。C. Hydrolysis rate of phosphamidon in alkaline solution(pH 9) was 2~4 times faster than that in acidic solution(pH 4) and neutral solution(pH 7) under same temperature. Hydrolysis rate constants of profenofos in pH 4, pH 7, and pH 9 buffer solutions at 25 and 40。C were 0.0022, 0.0047, 0.0860 and 0.0035, 0.0086, 0.1245, respectively. Hydrolysis rate of profenofos was accelerated by temprerature change under same pH conditions. Hydrolysis rate of profenofos in alkaline solution(pH 9) was 15~40 times faster than in acidic solution(pH 4) and neutral solution(pH 7) under same temperature condition, and half-life of profenofos was very fast within 8 hours. The hydrolysis rate of profenofos was faster than that of phosphamidon. In order to identify hydrolysis products, the extracts of degradation products were analyzed by GC/MS. The mass spectra of hydrolysis products of phosphamidon were at m/z 153 and 149, those of the profenofos were at m/z 208 and 240, respectively. The hydrolysis products of phosphamidon were O, O-dimethyl phosphate(DMP) and N, N-diethylchloroacetamide, and those of profenofos were 4-bromo-2-chlorophenol and O-ethyl-S-propyl phosphate.

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Determination and Monitoring of Grayanotoxins in Honey Using LC-MS/MS (LC-MS/MS를 이용한 벌꿀 중 grayanotoxin 분석법 연구 및 실태조사)

  • Lee, Sook-Yeon;Choi, Youn-Ju;Lee, Kang-Bong;Cho, Tae-Yong;Kim, Jin-Sook;Son, Young-Wook;Park, Jae-Seok;Im, Sung-Im;Choi, Hee-Jung;Lee, Dong-Ha
    • Korean Journal of Food Science and Technology
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    • v.40 no.1
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    • pp.8-14
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    • 2008
  • This study was performed to establish analysis methods, and evaluated for grayanotoxin in domestic/foreign honey and wild honey. The molecular weight of grayanotoxins I, II and III, excluding grayanotoxin III that has been commercialized, were analyzed by LC-MS/MS. Then, the molecular structure of grayanotoxins I and II were analyzed by NMR. A total 111 samples (25 Korean honey, 21 Korean wild honey, 13 Korean honeycomb honey, 44 foreign honey, 8 foreign wild honey) were examined to determined whether or not each sample contained grayanotoxins I, II, and III. The honey samples were mixed with methanol and loaded into a tC18 cartridge, the filtrate was diluted with water, and the mixture was then analyzed by ESI triple-quadrupole LC-MS/MS. Grayanotoxins were only found in the foreign wild honey and were not detected in Korean honey, Korean honeycomb honey, or Korean wild honey. Three of the samples contained grayanotoxin I, II, and III, and one sample contained only grayanotoxins I and III. The lowest level for grayanotoxin I was 3.13 ${\pm}$ 0.00 mg/kg, and the highest level was 12.93 ${\pm}$ 0.01 mg/kg. The levels of grayanotoxin II were 0.84 ${\pm}$ 0.01 mg/kg, 0.92 ${\pm}$ 0.00 mg/kg and 1.08 ${\pm}$ 0.01 mg/kg, respectively. The lowest level of grayanotoxin III was 0.25 ${\pm}$ 0.01 mg/kg and the highest level was 3.29 ${\pm}$ 0.74 mg/kg. Through this study, safety management for foreign wild honey has been enabled.