• Title/Summary/Keyword: Solid-phase

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Determining Anti-impotence drug-like compounds in Food (식품 중 발기부전치료제 및 유사물질의 분석)

  • Choi, Dongmi;Im, Mooheg;Lee, Kyungjin;Kwon, Kwangil;Jeong, Jiyoon;Park, Gunsang;Hong, Mooki;Lee, Chulwon
    • Analytical Science and Technology
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    • v.17 no.6
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    • pp.520-526
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    • 2004
  • To determine 6 anti-impotence drug-like compounds such as sildenafil, vardenafil, tadalafil, homosildenafil, hydroxyhomosildenafil and hongdenafil in food, simultaneously, high performance liquid chromatography was applied. In the case of solid sample, it was extracted in organic solvents after homogenizing with mortar and pestle. Whereas liquid sample was just diluted in water and then extracted in organic solvents. Maximum lengths of UV for targets have been identified on photodiode array spectra. As results, vardenafil, hongdenafil, hydroxyhomosildenafil, sildenafil, homosildenafil, and tadalafil were eluted in order using $C_{18}$ column in acetonitrile containing phosphoric acid as the mobile phase. The maximum wavelength (${\lambda}_{max}$) was 216 nm for vardenafil, 233 and 282 nm for hongdenafil, 222 and 293 nm for hydroxyhomosildenafil, sildenafil and homosildenafil, and 284 nm for tadalafil. The overall recoveries were ranged from 95% to 109% and the limit of detection was about 0.04 mg/kg at signal/noise>3. Levels of targets in the selected food samples were 1.7 (hongdenafil) ~ 63 (tadalafil) mg/one dose.

Development and validation of analytical methods for pyrifluquinazon residues determination on agricultural commodities by HPLC-UVD (HPLC-UVD를 이용한 농산물 중 pyrifluquinazon 잔류시험법 개발 및 검증)

  • Do, Jung-Ah;Kwon, Ji-Eun;Kim, Mi-Ra;Lee, Eun-Mi;Kuk, Ju-Hee;Cho, Yoon-Jae;Chang, Moon-Ik;Kwon, Kisung;Oh, Jae-Ho
    • Analytical Science and Technology
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    • v.26 no.3
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    • pp.174-181
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    • 2013
  • Pyrifluquinazon is classified with a quinazoline insecticide that regulates food intake by controling the feeding behavior acting on the endocrine or nervous system of pests such as aphids and white fly. To keep safety on pyrifluquinazon residues in agricultural commodities a simple, accurate and rapid analytical method was developed and validated using high performance liquid chromatograph (HPLC-UVD). The pyrifluquinazon residues acidified with 1% formic acid in samples were extracted with acetonitrile and partitioned with hexane subsequently to dichloromethane then purified with silica solid phase extraction (SPE) cartridge. The purified samples were detected using HPLC-UVD. The method was validated using apple and pear spiked with pyrifluquinazon at 0.02, 0.05 and 0.1 mg/kg and hulled rice, pepper, soybean at 0.05 and 0.1 mg/kg. Average recoveries were 70.5~107.9% with relative standard deviation less than 10%. The result of recoveries and overall coefficient of variation of a laboratory results in Gwangju regional FDA and Daejeon regional FDA was followed with Codex guideline (CODEX CAC/GL 40). This method is appropriated at pyrifluquinazon residues determination and will be used as official method of analysis.

Investigation of Nonylphenols Contamination in Solvents and Solid-phase Extraction Cartridge, and its Removal Protocols (정밀분석용 용매 및 SPE의 Nonylphenols 오염평가 및 제거)

  • Park, Jong-Min;Choi, Geun-Hyonng;Kim, Jung-Im;Hong, Su-Myeong;Kwon, Oh-Kyung;Im, Geon-Jae;Kim, Jin-Hyo
    • The Korean Journal of Pesticide Science
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    • v.15 no.1
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    • pp.22-27
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    • 2011
  • Nonylphenols are toxic compounds classified as endocrine disruptors. We investigated the nonylphenols clean-up procedures for the contamination control in the quantitative analysis. In this research we analyzed the residual nonylphenols in the solvent and the SPE cartridges. First, at the analysis of HPLC grade solvents (n-hexane, diethyl ether, ethyl acetate and its mixture), diethyl ether was confirmed the residue as 0.963 ${\mu}g/mL$, and we eliminated the contaminant through the distillation with $CaH_2$, Second, at the analysis of SPE cartridges (silica gel and Florisil), all products were showed the residue at 0.046~13.0 ${\mu}g/mL$, but unfortunately the residue in the cartridge were not easily removed with referenced methods in all tested SPE cartridges except in silica gel SPE cartridge with glass ware.

Monitoring of Neonicotinoid Pesticide Residues in Paprika Using UPLC-MS/MS from Gyeongnam Region (UPLC-MS/MS를 이용한 경남지역 파프리카 중 neonicotinoid계 농약 잔류 모니터링)

  • Kim, Nam-Kuk;Lee, Seung-Hwa;Nam, Yu-Jeong;Moon, Kyung-Mi;Park, Min-Ho;Yun, Mun-Hee;Kim, Mi-Young;Jang, Hyun-Min;Shin, Bong-Shig
    • The Korean Journal of Pesticide Science
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    • v.15 no.1
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    • pp.15-21
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    • 2011
  • Monitoring or follow-up surveying pesticide residues in agricultural commodities is the key to meet the international regulations and to enhance international competitiveness of Korean agricultural commodities. Six neonicotinoid insecticides, acctamiprid, clothianidin, dinotefuran, imidacloprid, thiacloprid, and thiamethoxam were monitored in 95 paprika samples collected from Gyeongnam area. Thc pesticide residues were extracted by EN 15662 buffer based on the QuEChERS method, clean-upped with dispersive solid-phase extraction method to remove interfering pigments, and analyzed using UPLC-MS/MS. The neonicotinoid pesticides were detected in 90.5% of the paprika samples. Two or more pesticides were detected in 82.3% of samples. Although detection frequencies were high, all samples complied with the maximum residue limits (MRLs) set by both the Korea Food and Drug Administration (KFDA) and Japanese Ministry of Health, Labour and Welfare.

A study on the electrodeposition of uranium using a liquid cadmium cathode at 440℃ and 500℃ (440℃와 500℃에서 액체카드뮴음극을 이용한 우라늄 전착에 관한 연구)

  • Yoon, Jong-Ho;Kim, Si-Hyung;Kim, Gha-Young;Kim, Tack-Jin;Ahn, Do-Hee;Paek, Seungwoo
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.11 no.3
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    • pp.199-206
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    • 2013
  • Electrowinning process in pyroprocessing recovers U (uranium) and TRU (Trans Uranium) elements simultaneously from spent fuels using a liquid cadmium cathode (LCC). When the solubility limit of U deposits over 2.35wt% in Cd, U dendrites were formed on the LCC surface during the electrodeposition at $500^{\circ}C$. Due to the high surface area of dendritic U, the deposits were not submerged into the liquid cadmium pool but grow out of the LCC crucible. Since the U dendrites act as a solid cathode, it prevents the co-deposition of U and TRUs. In this study, the electrodeposition of U onto a LCC was carried out at 440 and $500^{\circ}C$ to compare the morphology and component of U deposits. The U deposits at $440^{\circ}C$ have a specific shape and were stacked regularly at the center of the LCC pool, while the U dendrites (i.e., ${\alpha}$-phase) at $500^{\circ}C$ were grow out of the LCC crucible. Through the microscopic observation and XRD analysis, the electrodeposits at $440^{\circ}C$, which have a round shape, were identified as an intermetallic compound such as $UCd_{11}$. It can be concluded that the LCC electrowinning operation at $440^{\circ}C$ achieves the co-recovery of U and TRU without the formation of U dendrites.

High rate deposition of poly-si thin films using new magnetron sputtering source

  • Boo, Jin-Hyo;Park, Heon-Kyu;Nam, Kyung-Hoon;Han, Jeon-Geon
    • Proceedings of the Korean Vacuum Society Conference
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    • 2000.02a
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    • pp.186-186
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    • 2000
  • After LeComber et al. reported the first amorphous hydrogenated silicon (a-Si: H) TFT, many laboratories started the development of an active matrix LCDs using a-Si:H TFTs formed on glass substrate. With increasing the display area and pixel density of TFT-LCD, however, high mobility TFTs are required for pixel driver of TF-LCD in order to shorten the charging time of the pixel electrodes. The most important of these drawbacks is a-Si's electron mobiliy, which is the speed at which electrons can move through each transistor. The problem of low carier mobility for the a-Si:H TFTs can be overcome by introducing polycrystalline silicon (poly-Si) thin film instead of a-Si:H as a semiconductor layer of TFTs. Therefore, poly-Si has gained increasing interest and has been investigated by many researchers. Recnetly, fabrication of such poly-Si TFT-LCD panels with VGA pixel size and monolithic drivers has been reported, . Especially, fabricating poly-Si TFTs at a temperature mach lower than the strain point of glass is needed in order to have high mobility TFTs on large-size glass substrate, and the monolithic drivers will reduce the cost of TFT-LCDs. The conventional methods to fabricate poly-Si films are low pressure chemical vapor deposition (LPCVD0 as well as solid phase crystallization (SPC), pulsed rapid thermal annealing(PRTA), and eximer laser annealing (ELA). However, these methods have some disadvantages such as high deposition temperature over $600^{\circ}C$, small grain size (<50nm), poor crystallinity, and high grain boundary states. Therefore the low temperature and large area processes using a cheap glass substrate are impossible because of high temperature process. In this study, therefore, we have deposited poly-Si thin films on si(100) and glass substrates at growth temperature of below 40$0^{\circ}C$ using newly developed high rate magnetron sputtering method. To improve the sputtering yield and the growth rate, a high power (10~30 W/cm2) sputtering source with unbalanced magnetron and Si ion extraction grid was designed and constructed based on the results of computer simulation. The maximum deposition rate could be reached to be 0.35$\mu$m/min due to a high ion bombardment. This is 5 times higher than that of conventional sputtering method, and the sputtering yield was also increased up to 80%. The best film was obtained on Si(100) using Si ion extraction grid under 9.0$\times$10-3Torr of working pressure and 11 W/cm2 of the target power density. The electron mobility of the poly-si film grown on Si(100) at 40$0^{\circ}C$ with ion extraction grid shows 96 cm2/V sec. During sputtering, moreover, the characteristics of si source were also analyzed with in situ Langmuir probe method and optical emission spectroscopy.

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Kinetic Study of Cadmium Adsorption by Sewage Sludge (하수오니에 의한 Cd 흡착의 속도론적 연구)

  • Lee, Sang-Mo;Goh, Tee-Boon
    • Korean Journal of Soil Science and Fertilizer
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    • v.33 no.1
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    • pp.32-39
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    • 2000
  • To investigate the adsorption-desorption reaction of Cd by sewage sludge, the adsorption of Cd from $Cd(NO_3)_2$ solutions of concentrations ranging from 5 to $50{\mu}g\;Cd\;mL^{-1}$ by sewage sludge was examined for reaction periods up to 48 hours. The amount of Cd adsorbed as a function of time was measured. The adsorption between Cd in solution and the solid phase could be described by two stages. The initial adsorption of Cd was very rapid, that is, approximately 95% of the added Cd was removed from solution within the first 30 minutes. Further, the greater the concentration of Cd added, the greater was the amount of Cd adsorbed. After the rapid initial decrease of Cd, a slower decline in the Cd concentration resulted which followed first order reversible kinetics. The equilibrium concentrations for the reactions, as well as the time period for the equilibrium reactions were dependent on the initial Cd concentrations. If equilibrium is reached, the amount of Cd remaining in solution is greater when the amount adsorbed is higher, although the percentage of Cd in solution is constant relative to the initial concentration of Cd. Some of the adsorbed Cd was released back to solution since the concentration of Cd after 48 hours was higher than the equilibrium concentration of Cd. However, despite the increased amount of Cd measured, the overall net reaction was a significant adsorption of Cd from solution by sewage sludge.

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Mobilization Characteristics of Indigenous Phosphate by Oxalic Acid and Dilution Factors in Upland Soils (밭토양에서 옥살릭산과 희석요인에 의한 자체 인산의 이동 특성)

  • Chung, Doug-Young;Lee, Kyo-Suk
    • Korean Journal of Soil Science and Fertilizer
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    • v.39 no.1
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    • pp.46-51
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    • 2006
  • Phosphorus accumulation in fertilized soils becomes serious problem for agriculture and the environment. In this investigation, we conducted a laboratory scale investigation to find the most desirable displacement methods of the adsorbed phosphate onto the soil particle surfaces. Soil samples which contained high amount of phosphate were collected at two different depths (0-10 cm and 10-20 cm) from four locations at the moderate highland located in Nonsan, Chungnam. To observe the mobilization of solid-phase phosphate, soil samples were equilibrated with oxalic acid solutions ranging from $10^{-5}$ to $10^{-1}cmol\;L^{-1}$ with the dilution factors of 1:1, 1:2.5, 1:5, 1:10, and 1:20. The mineralized P sharply increased as the concentration of oxalic acid was greater than $5{\times}10^{-4}cmol\;L^{-1}$ under dilution factors of 1:1, 1:2.5, and 1:5. The breaking concentration of oxalic acid was lowered to $10^{-4}cmol\;L^{-1}$ and $5{\times}10^{-5}cmol\;L^{-1}$ for dilution factors of 1:10 and 1:20, respectively. The curve fit obtained from the graph can be described by exponential growth when the dilution factors were 1:1, 1:2.5, and 1:5 while the sigmoidal shape for 1:10 and 1:20, showing the mineralization of P were significantly dependent on the dilution factor.

Improvement of Growth and Soil Environment by Topdressing and Tillage in Zoysiagrass (Zoysia japonica) Cultivation Field (잔디 재배지에서 배토와 경운처리에 의한 잔디생육 및 토양환경 개선)

  • Han, Jeong-Ji;Choi, Su-Min;Lee, Kwang-Soo;Park, Yong-Bae;Bae, Eun-Ji
    • Weed & Turfgrass Science
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    • v.5 no.3
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    • pp.165-169
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    • 2016
  • To establish the soil management system for the efficient sod production, survey on the growth of zoysiagrass by different soil managements was conducted in repeated cultivation field with regard to soil physical properties. Soils were subjected to four types of management methods, which include (1) rolling (2) topdressing (3) topdressing + rolling (4) topdressing + tillage + rolling. The topdressing + tillage + rolling treatment significantly ameliorated soil physical properties such as bulk density, porosity and solid phase as compared to rolling and topdressing + rolling treatments, and was not significantly different from the topdressing treatment. Further growth and density of zoysiagrass except for the root dry weight in topdressing + tillage + rolling treatment were significantly higher than that only in rolling treatment. Topdressing + tillage + rolling treatment significantly increased the number of shoot as compared to the other treatments. Therefore, combined topdressing and tillage soil management practice should be conducted for the production of zoysiagrass in repeated cultivation field.

Herbicidal Activity of Essential Oil from Palmarosa (Cymbopogon martini) (팔마로사 정유의 살초활성)

  • Hong, Su-Young;Choi, Jung-Sup;Kim, Song-Mun
    • Korean Journal of Weed Science
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    • v.31 no.1
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    • pp.96-102
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    • 2011
  • The objective of this study was to find herbicidal compounds in the essential oil of palmarosa (Cymbopogon martini). Of essential oils from basil (Ocimum basilicum), blackpepper (Piper nigrum), clary sage (Salvia sclarea), ginger (Zingiber pfficinale), hyssop (Hyssopus officinalis), nutmag (Myristica fragrance), palmarosa (Cymbopogon martini), fennel (Foeniculum vulgare), sage (Salvia leucantha), and spearmint (Mentha spicta), the herbicidal activity of palmarosa essential oil, which was determined by a seed bioassay using rapeseed (Brassica napus L.), was highest ($GR_{50}$ value, $201{\mu}g\;mL^{-1}$). In palmarosa essential oil, 11 volatile organic chemicals were identified by gas chromatography-mass spectometry with solid-phase micro-extraction apparatus and the major constituents were geraniol (40.23%), geraniol acetate (15.57%), cis-ocimene (10.79%), and beta-caryophyllene (8.72%). The $GR_{50}$ values of geraniol, citral, nerol, and geranyl acetate were 151, 224, 452, and $1,214{\mu}g\;mL^{-1}$, respectively. In greenhouse and field experiments, foliar application of palmarosa essential oil at the level of $80kg\;ha^{-1}$ controlled weeds effectively. Overall results of this study showed that the herbicidal activity of palmarosa essential oil could be due to geraniol and citral which had lower $GR_{50}$ values.