• Title/Summary/Keyword: solvent recovery

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Evaluation of Testosterone Metabolites/Dehydroepiandrosterone As the Indicators of Testosterone Administration in Horse Doping (경주마 약물검사에서 testosterone 투여 여부표지자로서의 testosterone 대사체들에 대한 dehydroepiandrosterone의 비율 평가)

  • Kim, Jin Young;Choi, Man Ho;Kim, Sung Jean;Kyong, Jin Burm;Chung, Bong Chul
    • Analytical Science and Technology
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    • v.12 no.3
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    • pp.190-195
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    • 1999
  • The metabolism of testosterone ($17{\beta}$-hydroxy-androst-4-en-3-one) was confirmed in horse after a single intramuscular administration of testosterone cypionate (750 mg). Solvent extracts of urine obtained with enzymatic hydrolysis and methanolysis were analyzed by GC/MS after oxime t-butyldimethylsilyl (oxime-TBDMS) derivatization. The structures of four urinary metabolite after testosterone administration in horse were determined based on EI mass spectra and $5{\alpha}$-androstane-$3{\beta}$, $17{\alpha}$-diol and $5{\alpha}$-androstane-$3{\beta}$-ol-17-one as major was confirmed with authentic standard. Also the concentrations of $5{\alpha}$-androstane-$3{\beta}$, $17{\alpha}$-diol, $5{\alpha}$-androstane-$3{\beta}$, $17{\beta}$-diol, dehydroepiandrosterone (DHEA), $5{\alpha}$-androstane-$3{\beta}$-ol-17-one and testosterone were determined in the urine of normal subjects and the urine after administration. The recovery and detection limit in the most drugs were 86.3~94.7% and 1~3 ppb, respectively. Correlation coefficients for calibration were in the range of 0.984~0.999. Excretion profile of testosterone presents the rapid and large increasement up to maximum values at days 5 after administration and the slow regression. The relative ratios of testosterone, its metabolites over DHEA were determined for indication of testosterone administration in horse doping.

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Quantitative Determination of Phenol in Water Using GC-MS after Liquid-Liquid Extraction and Acetylation (액-액 추출과 아세틸화 후 GC-MS를 이용한 물 중 phenol의 분석)

  • Park, Sunyoung;Kim, Yunjeong;Jung, Sungjin;Kim, Hekap
    • Korean Journal of Environmental Agriculture
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    • v.36 no.1
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    • pp.63-66
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    • 2017
  • BACKGROUND: The phenol concentrations in water samples were determined using gas chromatography after derivatization of the analyte to phenyl acetate followed by extraction using a large volume of solvent. However, this procedure requires an additional purification step and is not analytically efficient. METHODS AND RESULTS: In this study, phenol was first extracted from an acidified water sample using ethyl acetate and then acetylated using acetic anhydride in the presence of a small amount of water and $K_2CO_3$. The derivative was extracted using 1mL of n-butyl acetate. One microliter of the extract was analyzed by GC-MS without further purification. The calibration curve showed good linearity with the $r^2$ value of 0.9968. The method detection limit and the limit of quantitation were estimated to be $0.18{\mu}g/L$ and $0.56{\mu}g/L$, respectively. Repeatability (RSD, n=3) and recovery (n=3) were 9.1%-4.3% and 90.6%-110.5%, respectively. The concentrations of phenol in a few samples of stream water were distributed in the range of $2.51-7.51{\mu}g/L$. CONCLUSION: This method is simpler and faster to implement than those currently utilized and shows high analytical reliability. It can be applied to the quantitative determination of phenol concentrations in surface water and groundwater samples.

Determination of Ethylenethiourea in Fruits (과실류에 잔류하는 Ethylenethiourea 분석)

  • Kim, Eun-Hee;Jang, Mi-Ra;Kim, Jin-A;Kim, Tae-Rang;Yook, Dong-Hyun;Hwang, In-Sook;Kim, Jung-Hun
    • Korean Journal of Food Science and Technology
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    • v.43 no.3
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    • pp.277-281
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    • 2011
  • A rapid and very sensitive high-performance liquid chromatography/atmospheric-pressure chemical-ionization mass spectrometry method to detect ethylenethiourea (ETU) fungicide residues in fruits was developed. Methylene chloride was used as the surface extraction solvent for the target component. Recovery rates improved when cysteine hydrochloride and sodium carbonate were added to product prior to fortification. The limits of detection and quantification were approximately 0.006 and 0.02 mg/kg, respectively, from mandarin oranges. Recoveries from mandarin oranges, oranges, bananas, and pears, spiked in the range of 0.05-0.5 mg/kg, averaged 80-100%. The proposed method was used to monitor the presence of ETU in commercial fruits purchased from different markets in Seoul, Korea. ETU was found in four orange peels and in three mandarin orange peel samples. The highest ETU residue levels were $73.6{\mu}g/kg$ and $29.8{\mu}g/kg$.

A Study on the Classifying Quality Standard by Comparison with Physicochemical Characteristics of Virgin, Pure, Pomace Olive Oil (버진, 퓨어, 포마스 올리브유의 이화학적인 특성 비교를 통한 품질등급 구분에 관한 연구)

  • Cho, Eun-Ah;Lee, Young-Sang
    • The Korean Journal of Food And Nutrition
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    • v.27 no.3
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    • pp.339-347
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    • 2014
  • This study investigated the classification of olive oils that are mainly distributed in Korea via imports. The fatty acid contents, degree of color, pigments, anti-oxidants, and sterol contents are analyzed on the different types of olive oil as follows: 10 kinds of extra virgin olive oil, 5 kinds of pure olive oil, and 5 kinds of refined olive-pomace oil. As a result of fatty acid analysis, the majority of oleic acid ($C_{18:1}$) and palmitic acid ($C_{16:0}$), and minority of linoleic acid ($C_{18:2}$) and stearic acid ($C_{18:0}$) were detected without any significant differences between the grades of olive oils. The UV spectrum is related to the ${\Delta}K$, and it is a part of the analysis factor for the purity and degree of degradation of the oil. Extra virgin olive oil had ${\Delta}K$ of almost 0, pure olive oil had 0.07~0.12, and refined olive-pomace oil had 0.1~0.13. These differed from extra virgin oil, and the pure or pomace oil ${\Delta}K$ had a confirmed distinct difference. The color degrees of chlorophyll with a low $L^*$ value and $(-)a^*$ (green) and carotenoid with $(+)b^*$ (yellow) were confirmed to have correlation between extra virgin and other olive oils. To compare chlorophyll and carotenoid as natural pigment in olive oils, 417 nm and the ratio of the absorbance at 480 nm (417/480) was calculated at 1.62 of extra virgin, 1.85 of pure olive oil, and 3.32 of refined olive-pomace oil. Therefore, it will be possible to distinguish when the extra virgin or pure olive oil are mixed with olive-pomace oil. The total amount of tocopherol, an anti-oxidant, were 19.06 in extra virgin, 10.91 in pure olive oil, and 27.88 in refined olive-pomace oil. The high content of tocopherol in pomace oil caused recovery of solvent extraction from olive pulp. Thus, extra virgin oil and pure olive oil were distinguished by olive-pomace oil. Polyphenol compounds in extra virgin olive oil measured high only in ferulic acid with 0.543 mg/kg, caffeic acid with 0.393 mg/kg, and other vanillic acid, vanillin, and p-coumaric acid had similar amount of 0.3 mg/kg. All grade of olive oils had the highest ${\beta}$-sitosterol content. Af (Authenticity factor) value were estimated with campesterol and stigmasterol content ratio (%). Af value was 19.2 in extra virgin olive oil, 17.1 in pure olive oil, 16.9 in refined olive-pomace oil, which were distinctive from sunflower oil with 3.7, corn oil with 2.4, and soybean oil with 2.0. It can provide important indicator of olive oil adulteration with other cheap vegetable oils. The results of this study can be used as a database for the classification of olive oil grade and distinguishing between the different types of oils.

The Effect of Residual Water on the Adsorption Process of Carbon Tetrachloride by Activated Carbon Pellet (활성탄에 의한 사염화탄소 흡착공정에서 잔존수분의 영향)

  • Jeong, Sung Jun;Lee, Dae Lo;Kim, Tae Young;Kim, Jin Hwan;Kim, Seung Jai;Cho, Sung Young
    • Korean Chemical Engineering Research
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    • v.40 no.6
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    • pp.694-702
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    • 2002
  • Activated carbons have been used as adsorbents in various industrial application, such as solvent recovery, gas separation, deodorization, and catalysts. In this study, the effects of residual water on the activated carbon adsorbent surface on the adsorption capacity of $CCl_4$ were investigated. Adsorption behavior in a fixed bed was studied in terms of feed concentration, flow rate, breakthrough curve and adsorption capacity for $CCl_4$. Desorption characteristics of residual water on activated carbon were also studied. The water contents of the activated carbon were varied in the range of 0-20%(w/w) and all experiments were performed at 298.15 K. The adsorption equilibrium data $CCl_4$ on the activated carbon were well expressed by Langmuir isotherm. The adsorption capacity of $CCl_4$ decreased with increasing residual water content. Desorption of residual water in activated carbon decreased expotentially with $CCl_4$ adsorption. The obtained breakthrough curves using LDF(linear driving force) model represented our experimental data.

Determination of Aldehydes in Tap Water by Reverse Phase Liquid Chromatography (역상 액체 크로마토그래피에 의한 수도수 중 알데하이드류의 정량)

  • Choi, Yong Wook;Choi, Yun Jung
    • Journal of the Korean Chemical Society
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    • v.43 no.4
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    • pp.438-446
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    • 1999
  • The optimum analytical method of aldehydes, ozone by-products, was established by reverse phase liquid chromatography. Six aldehydes including formaldehyde, acetaldehyde, acrolein, propionaldehyde, butylaldehyde and benzaldehyde, and one ketone including acetone were selected as aldehyde test samples through preliminary experiments. Such analytical conditions as the pH of citrate buffer solution, reaction temperature, reaction time, and concentration of DNPH, the component and composition of desorption solvent were optimized. As the result, pH 3.0 of citrate buffer solution, 40$^{\circ}C$ of reaction temperature, 15 minutes of reaction time, and 0.012% of DNPH concentration were chosen as optimum conditions. Aldehydes-DNPH derivatives in water were concentrated on $C_18$ Sep-Pak cartridge and followed by elution of their derivatives fraction with THF/ACN(70/30) mixture, and showed recoveries of the range from 87 to 107%. Separation condition on Nova-Pak $C_18$ column with low pressure gradient elution from ACN/MeOH/water(30/10/60) of an initial condition to 80% ACN of a final condition was found to give a good resolution within 20 minutes of run time. 86% to 103% of recovery for aldehydes using this method was similar to that for aldehyde using EPA Method 554 which is ranged from 84% to 103%.

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Extraction of Intracellular Lipids from Recombinant E. coli for Improving Long-chain Fatty Acid Production (긴 사슬 지방산 생산을 위해 재조합된 E. coli로부터의 세포 내 지질 추출)

  • Ham, Su Mi;Yoo, In Sang;Park, Sang Joon;Kim, Ji Hyeon
    • Korean Chemical Engineering Research
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    • v.51 no.4
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    • pp.482-486
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    • 2013
  • Recently, biohydrocarbons are gathering an interest as a new bioenergy due to the versatile applicability. In the present work, a process is proposed for the recovery of lipids from Recombinant E. coli MG1655 which provides longer chain fatty acids. After the growth of the recombinant E. coli, the cells were disrupted by high pressure homogenizer for obtaining intracellular lipids and the resulting solutions were centrifuged and extracted. For the efficient cell disruption with high pressure homogenizer, the pressure higher than 5,000 psi was required. In addition, under the conditions of applied pressure 5,000 to 20,000 psi, 1~3 pass homogenizing was enough for the more than 90% cell disruption. As organic solvents for extraction of lipid, hexane/isopropyl alcohol and ethyl acetate/ethanol systems showed excellent extracting power. With these solvent systems, the 60% lipid could be recovered. Moreover it was found that the extracted lipids contained long-chain fatty acids such as $C_{12}$, $C_{14}$, $C_{16}$ and $C_{18}$.

Determination of PFOS in LDPE and the Result for Proficiency Testing (LDPE 중 PFOS의 분석법 개발과 비교숙련도 결과)

  • Jung, Jae Hak;Lee, Young Kyu;Myung, Seung Woon;Cheong, Nam Yong
    • Journal of the Korean Chemical Society
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    • v.57 no.1
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    • pp.40-51
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    • 2013
  • In order to develop a quantitation method for Perfluorooctanesulfonic acid(PFOS) contained in plastics that are mainly used in electric and electronic equipment, this study consisted of conducting method validations with LDPE samples using soxhlet solvent extraction and LC/MS. As a result, the limits of detection and quantitation (LOD, LOQ) were $2.58{\mu}g/L$ and $7.82{\mu}g/L$, respectively. Additionally, the recovery was 96-102%. For the correlation coefficient of LC/MS, the $r^2$ value was 0.9992 in the concentration range of $7.82-100{\mu}g/L$, which confirmed its linearity. Furthermore, for the standardization of the analysis method for PFOS in electric and electronic equipment to correspond to EU environmental regulations, we conducted a proficiency test with a number of domestic and international testing laboratories. Three of the ten testing laboratories that participated in the proficiency test submitted outliers. Accordingly, we examined the cause of the outliers using the $^{19}F$ NMR, finding that the main cause was an error in the processing of the results for isomers in PFOS that existed in standard solutions and samples.

Determination of Di-(2-Ethylhexyl) Adipate Migrated from Polyvinyl Chloride Wrap Film into Various Foodstuffs and Dishes Depending on Exposure Conditions (염화비닐 랩 필름으로 포장된 다양한 식품 및 요리류의 노출 조건에 따른 di-(2-ethylhexyl) adipate의 이행량 분석)

  • Lee, Young-Ho;Gyoung, Young-Soo;Lee, Keun-Taik
    • Korean Journal of Food Science and Technology
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    • v.34 no.6
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    • pp.969-976
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    • 2002
  • The migrating level of di-(2-ethylhexyl) adipate (DEHA) in PVC wrap to various foodstuffs dishes was determined using acetone/n-hexane as an extracting solvent. The recovery ratio of DEHA from various foodstuffs ranged from 81.3 to 91.2%. During storage at $10\;or\;20^{\circ}C$ for up to 3 days, highest migration of 22.9 mg/kg occurred with pork belly, an indication that increases in fat content, storage temperature, and storage time result in increasing DEHA migration. DEHA concentrations of various delivered dishes ranged between 6.9 and 29.8 mg/kg, and highest migration was observed in Chambbong, which had the highest fat content among samples. After microwave-reheating, which resulted in a tight contact between film and food samples, DEHA was not detected in rice and potato, whereas up to 158.8 mg/kg was detected in pizza. When the wrap film was not contacted with the surface of food, the migration was lowered. Migration levels of DEHA from PVC wrap film into samples under various exposure conditions often exceeded the limit value of $3\;mg/dm^2\;and/or\;18\;mg/kg$ set by the European Union.

Why did she lose her sight? A case of visual damage due to methanol inhalation (메탄올 흡입 후 발생한 시각장애 : 증례보고)

  • Han, Sangsoo;Shin, Hee-Jun
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.19 no.11
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    • pp.421-425
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    • 2018
  • Methanol is a clear, colorless, volatile, and poisonous liquid that is commonly used as an industrial solvent. Visual impairment is a common symptom of methanol poisoning; however, visual impairment rarely occurs after exposure through inhalation. Therefore, visual loss after methanol intoxication via respiration has rarely been reported. We report a case of visual damage associated with methanol poisoning via respiratory exposure in an industrial setting. In this case in South Korea, a 28-year-old woman who worked at a cell phone factory was admitted to the emergency department with mental changes. She had blurred vision that began two days prior, but she did not come to the hospital until she experienced mental changes. She ranked 9 on the Glasgow Coma Scale and presented with severe metabolic acidosis. So, she was admitted to intensive care, and continuous renal replacement therapy was performed. Finally, she was discharged after recovery of her mental state, but had to undergo rehabilitation for six months. Also, her visual impairment was permanent. Methanol intoxication can occur through inhalation, which is difficult to detect initially. However, treatment of methanol poisoning is time-critical. Therefore, doctors should always keep in mind that methanol intoxication may occur via respiration. If in doubt, treatment should be given as soon as possible.