• Title/Summary/Keyword: recoveries

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Recovery Behaviors of Natural Rubber Composites Thermally Aged in Altering Medium Systems of Air and Water (공기와 물의 교매질 시스템에서 열노화된 천연고무 복합체의 회복 거동)

  • Choi, Sung-Seen;Kim, Ok-Bae
    • Elastomers and Composites
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    • v.48 no.3
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    • pp.181-189
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    • 2013
  • Unfilled, carbon black-filled, and silica-filled natural rubber (NR) composites were aged with a circular deformation at $60-90^{\circ}C$ and the recovery behaviors were investigated. The samples were aged under the altering aging medium systems of air and distilled water every day for 10 days. The order of the recoveries according to the filler systems was unfilled > silica > carbon black. The recoveries of the samples aged in the air to water altering system were greater than those of the samples aged in the water to air altering system. The initial aging medium dominantly influenced the deformation level.

Highly Selective and Simple Zero and First Order Derivative Spectrophotometric Determination of Palladium by Using α-Benzilmonoxime in Triton X-100 Micellar Solution

  • Eskandari, Habibollah;Karkaragh, Gholamhassan Imanzadeh
    • Bulletin of the Korean Chemical Society
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    • v.24 no.12
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    • pp.1731-1736
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    • 2003
  • The reaction of ${\alpha}$-Benzilmonoxime with palladium(II) produces a green complex in triton X-100 micellar media. Palladium has been determined using zero and first derivative spectrophotometric methods. The absorbances of Pd(II)- ${\alpha}$--benzilmonoxime complex at 441.8 and 677.0 nm in 0.10 M perchloric acid solution were monitored and linear working ranges of 0.3-12.0 and 0.7-20 ${\mu}$g mL$^{-1}$ with detection limits of 0.07 and 0.10 ${\mu}$g $mL^-1$ were obtained, respectively. Also, recoveries in the range of 92.8 to 100.1% and relative standard deviations in the range of 0.4 to 7.1% were obtained. First derivative spectrophotometry has also been applied for palladium determination under the optimum condition. The linear dynamic range of 0.2-24.0 ${\mu}$g $mL^{-1}$ palladium with relative standard deviations of 0.6-6.9% and recoveries in the range of 94.9-102.5% has been obtained by first derivative spectrophotometry. The method shows high selectivity because of the high concentration of acid used, which prevents formation of complexes of ${\alpha}$--benzilmonoxime with the other cations. The palladium complex formed was stable at least one day. The method was successfully applied to the determination of palladium in some synthetic palladium alloys and palladium-charcoal powder.

Simultaneous Determination of Anthraquinone, Flavonoids, and Phenolic Antidiabetic Compounds from Cassia auriculata Seeds by Validated UHPLC Based MS/MS Method

  • Girme, Aboli;Saste, Ganesh;Chinchansure, Ashish;Joshi, Swati;Kunkulol, Rahul;Hingorani, Lal;Patwardhan, Bhushan
    • Mass Spectrometry Letters
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    • v.11 no.4
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    • pp.82-89
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    • 2020
  • A systematic isolation and characterization study for Cassia auriculata (CA) seeds resulted in identifying antidiabetic compounds 1,3,8-trihydroxyanthraquinone and quercetin, quercetin-3-O-rutinoside, gallic acid, caffeic acid, ferulic acid, and ellagic acid. The ultra-high-performance liquid chromatography based triple quadrupole mass spectrometry methodology was developed and validated for simultaneous identification and confirmation of these compounds from CA seeds. Multiple reaction monitoring (MRM) based quantification method was developed with MRM optimizer software for MS1 and MS2 mass analysis. The method was optimized on precursor ions and product ions with the ion ratio of each compound. The calibration curves of seven bioactive analytes showed excellent linearity (r2 ≥ 0.99). The quantitation results found precise (RSD, < 10 %) with good recoveries (84.58 to 101.42%). The matrix effect and extraction recoveries were found within the range (91.66 to 102.11%) for the CA seeds. This is the first MS/MS-based methodology applied to quantifying seven antidiabetic compounds in CA seeds and its extract for quality control purposes.

Monitoring for fluoroquinolones residues in raw meat in Sejong (세종지역 유통 식육의 플루오로퀴놀론계 항생제 잔류 연구)

  • Jeong, Yoon-Kyung;Lee, Taeho;Lee, Jong Hoon;Kim, Mun-Bae
    • Korean Journal of Veterinary Service
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    • v.45 no.3
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    • pp.229-236
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    • 2022
  • This study describes an analytical method based on LC-MS/MS for the quantitation of 5 fluoroquinolones (Enrofloxacin, Ciprofloxacin, Marbofloxacin, Norfloxacin and Danofloxacin) in meat, and was applied to 230 meat samples for validation. Quantitation was performed based on a matrix-matched calibration to compensate for the matrix effect on the electrospray ionization. Good linear calibrations (R2≥0.998) were obtained for all fluoroquinolones at 6 concentrations of 1~50 ㎍/kg. Satisfied recoveries of all fluoroquinolones were demonstrated in spiked meat at three levels from 10 to 50 ㎍/kg. The recoveries ranged between 75.8~99.2% in beef, 80.1~99.6% in pork and 72.2~99.8% in chicken, respectively. The limits of quantitation (LOQs) for fluoroquinolones ranged from 0.7 to 3.2 ㎍/kg. We also monitored fluoroquinolones residue in the sample (beef 107, pork 71, chicken 52) using LC-MS/MS. Residues of fluoroquinolones which exceeded maximum residue limits (MRL) were not exceed in any of the 230 samples.

Radioactivity Analysis of $^{55}Fe\;and\;^{63}Ni$ in Dismantled Concrete (해체 콘크리트 폐기물에 포함된 $^{55}Fe$$^{63}Ni$ 방사능 분석)

  • Kang, Mun-Ja;Chung, Kun-Ho;Hong, Sang-Bum;Choi, Geun-Sik;Lee, Chang-Woo
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.5 no.1
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    • pp.19-27
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    • 2007
  • Combined method of extraction chromatography and liquid scintillation analysis was established for determinating $^{55}Fe\;and\;^{63}Ni$ radioactivity in solid samples. Activated concrete wastes generated from dismantling KRR-2 were analysed. The sequential separation including precipitation and extraction chromatography resulted in the above 90% chemical recoveries of Fe. Above 62% recoveries of Ni were obtained by this procedure exception to 43.6 and 46.5% recoveries. The seperation and counting procedure was also confirmed with spiked samples of known quantity. The measured and spiked quantity were agreed with the 3.7% and 0.7% variations in the $^{55}Fe\;and\;^{63}Ni$ experiments, respectively. The radioactivities of $^{55}Fe$ in the dismantled concretes are shown from below MDA to maximum 362 Bq/g. The radioactivities of $^{63}Ni$ in all concrete samples are below MDA. The $^{63}Ni$ doesn't exist in dismantled concretes from KRR-2. The radioactivity of $^{55}Fe$ is decreased rapidly as the sampling depth is increased from the concrete surface.

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Study on the Development of Simultaneous Analytical Method for the Residual Organic Chloride Pesticides by Gas Chromatography (기체 크로마토그래피를 이용한 유기 염소계 잔류 농약 동시 분석 방법 개발에 관한 연구)

  • Kim, Woo-Seong;Lee, Bong-Hun;Park, Heung-Jai
    • Journal of Environmental Science International
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    • v.5 no.5
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    • pp.561-567
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    • 1996
  • A method for the simultaneous analysis of 31 residual organic chloride pesticides was studied using gas chromatography. Prepared analytical samples were injected to gas chromatography (HP 5890 Series II plus) on the Ultra-2 column with ECD. The packing materials for column were changed as the following reagents ; florisil and alumina N, The residual solution was loaded to column and was elected pith erection solvents ; ether : benzene (2 : 8) solution, hexane : benzene (1 : 1) solution, dichloromethane, acetone, and methanol. The analytical results showed that 6 kinds of organic chlorides were not detected when florisil (first condition) was used as the column packing material. The nondetected 6 kinds of organic chlorides in the first analytical condition were detected and the recoveries of thrin-pesticides were increased, in particular, captan and captafol, but the recoveries of benzene hexachloride compounds were decreased when dichloromethane and methanol were added as elution solvents (pac'king material was florisil as in the first condition). The recoveries of dichlornuanid, chlorofenvinfos, folpet, and dicofol were increased and that of aldrin was increased, but those of captan and captafol were not good when alumina N was used as the packing material. To detect simultaneously thrin-pesticides, captan, and captafol, florisil and alumina N were used as the packing materials. The elution result showed that captan and captafol were not detected. This was because the column was activated insufficiently. The analytical method was the best (31 kinds of organic chlorides in the residual pesticides were detected sharply and showed high sensitivity) when the column (packing materials were florisil and alumina N: together) was fuliy activated and the impurities were removed using various elution solvents.

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Matrix solid phase dispersion isolation and high performance liquid chromatographic determination of five benzimidazole anthelmintics in bovine muscle, liver and omasum (시료고체상분산처리와 액체크로마토그라피를 이용한 소의 근육, 간 및 천엽에서의 벤지미다졸계 구충제 잔류분석)

  • Kim, Chung-Hui;Kim, Gon-Sup;Park, Jung-Hee;Hah, Dae-Sik;Ryu, Jae-Doo;Son, Sung-Gi;Heo, Jung-Ho;Jung, Myung-Ho;Kim, Jong-Shu
    • Korean Journal of Veterinary Research
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    • v.42 no.2
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    • pp.171-181
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    • 2002
  • Simultaneous multiresidue analysis using liquid chromatography determination for five benzimidazole anthelmintics(thiabendazole, oxibendazole, albendazole, mebendazole and fenbendazole) in bovine muscle, liver and omasum has been described. Blank or benzimidazole-fortified samples(0.5g) were blended with bulk $C_{18}$($40{\mu}m$, 18% load, endcapped, 2g). A column made from the resultant $C_{18}$/animal tissue matrix was first washed with hexane($8m{\ell}$), following which the benzimidazoles were eluted with acetonitrile($8m{\ell}$). Analytes of extracted sample were determined by liquid chromatography with UV detector at 290nm. Correlation coefficients of standard curves for individual benzimidazole isolated from fortified samples, using internal standardization, were linear($0.991{\pm}0.007$ to $0.996{\pm}0.005$) with average relative percentage recoveries from $62.1{\pm}3.8(%)$ to $92.3{\pm}7.5(%)$ for the concentration range($0.2{\sim}6.4{\mu}g/g$), respectively. Recoveries rates of TBZ, MBZ in liver, OBZ, MBZ in muscle and TBZ, MBZ in omasium from fortified benzimidazole were 92.%, 87.3%, 74.5%, 82.7%, 75.2% and 83.5% at condition II, respectively. Condition II showed higher recoveries rates than condition I. These results indicated that the matrix solid phase dispersion(MSPD) methodology is acceptable for the determination of 5 benzimidazole anthelmintics and may also suitable for other matrixes of food animal origin.

Mucosal Mast Cell Responses in the Small Intestine of C3H/HeN and BALB/c Mice Infected with Echinostoma hortense

  • Ryang, Yong-Suk;Im, Jee-Aee;Kim, In-Sik;Kim, Keun-Ha
    • Biomedical Science Letters
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    • v.9 no.3
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    • pp.145-150
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    • 2003
  • In the intestinal mucosa, mast cells are thought to be responsible for the expulsion of parasites. We investigated the relationship of worm expulsion and mast cells in C3H/HeN and BALB/c mice infected with Echinostoma hortense. In addition, we examined whether the worm recovery rate was associated with the strain of mice, and whether a toluidine stain and immunohistochemistry using the c-kit antibody was effective in the detection of mast cells. In order to investigate the mucosal immune response of C3H/HeN and BALB/c mice, each mouse was infected orally with 30 E. hortense metacercariae. Then, the number of mucosal mast cells and worm recovery rates was observed in experimentally infected mouse strains between 1 week and 8 weeks post infection (PI). Mucosal mast cells were increased in 3 weeks P.I. in C3H/HeN and BALB/c mice. On the other hand, only mucosal goblet cells and worm recovery rates correlated in C3H/HeN mice (P=0.0482). Worm recoveries in C3H/HeN mice were 65.7$\pm$5.6, 53.3$\pm$5.4 and 6.7$\pm$0.6 in week 1, 2, and 3 P.I. and strongly decreased in week 3 P.I. Worm recoveries in BALB/c mice were 23.0$\pm$2.5, 10.0$\pm$1.0, and 6.7$\pm$0.6% in week 1, 2, and 3 P.I. and gradually decreased from week 1 P.I. to week 3 P.I. Worm recoveries in C3H/HeN mice were significantly higher than in BALB/c mice (P<0.00l). The number of mast cells in C3H/HeN and BALB/c mice using the anti-c-kit antibody reached to a peak in week 3 P.I. and recovered as normal level in week 5 P.I. and 6 P.I. The number in E. hortense-infected C3H/HeN mice (P=0.0015) was higher than in E. hortense-infected BALB/c mice (P=0.01) compared with the control group. There were significant differences in the number of mast cells among regions of the intestine in in C3H/HeN mice (P<0.05) but not in BALB/c mice (P>0.05). Immunohistochemistry using the anti-c-kit antibody was significant method as an examination of the number of mast cells (P=0.0002). In conclusion, the present study demonstrated that mast cells play an important role in worm recovery, and immunohistochemistry using the anti-c-kit antibody was superior to toluidine stain as an examination of mast cells.

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Interlaboratory Study for Cryptosporidium and Giardia Test Methods in Water (정수장 원생동물 분석방법의 국내 실험실간 교차시험 연구)

  • Chung, Hyenmi;Park, Sangjung;Kim, Daekyun;Park, Sanghee;Kim, Reeho;Lee, Sangho;Cho, Joorae;Lee, Kyeunghee;Park, Jonggeun;Lee, Mokyoung;Byun, Seungheon;Cho, Eunju;Rhim, Yeontaek
    • Journal of Korean Society on Water Environment
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    • v.22 no.2
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    • pp.321-327
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    • 2006
  • This interlaboratory study was designed to evaluate protozoan test methods in water and to predict the major causes of deviation of the methods. Each of four laboratories with previous experience of protozoa analysis in water participated, and met the initial performance criteria of EPA 1623 method provided. The protozoan analysis procedure consists of filtrations, concentration, immunomagnetic separation, dyeing (staining) and counting with observation. We tested three different filtration equipments: capsule filter for 10 L of surface water, and high volume (HV) capsule filter and membrane filter for 100 L of finished water. When the recovery of each step of the procedure was evaluated with EasySeed, the commercial stock of each 100 Cryptosporidium and Giardia, immunomagnetic separation and filtration step were the most crucial steps affecting the stability of the recovery, especially for Cryptosporidium. There was no significant difference of recovery among the filtration methods. Recovery of protozoa from source water were evaluated with spiked EasySeed as matrix tests. The recoveries of Giardia increased significantly in the matrix tests compared those in the deionized water. We also applied red stained mixture stocks of Cryptosporidium and Giardia called ColorSeed as internal standards of water sample tests. The recoveries of both EasySeed and ColorSeed in samples tested were within the range of the criteria, however, the Giardia recoveries using ColorSeed decreased significantly. Further optimization study with ColorSeed will be necessary, considering the convenience of using the internal standard without additional sample analysis. The significant factors of the recovery variation were identified as the differences of laboratories as well as water quality and type of the stock for spiking. The results of this study emphasize the importance of the quality assurance program for protozoan analysis lab in water.

Extraction Efficiencies of Organophosphorus Pesticides Spiked in Fish Tissues by Supercritical Carbon Dioxide (초임계 이산화탄소에 의한 어류조직 중 유기인계 농약의 첨가회수율)

  • Lim, Sang-Bin;Jwa, Mi-Kyung
    • Korean Journal of Food Science and Technology
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    • v.30 no.5
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    • pp.1163-1168
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    • 1998
  • Fish tissues were spiked with organophosphorus pesticides (OPPs), mixed with a celite as a drying agent, and dynamically extracted with pure $CO_2$ or modified $CO_2$ for 10 min at different extraction temperatures, pressures and $CO_2$ flow rates. Recoveries of OPPs spiked in jacopever increased with the decrease of extraction temperature and pressure, and decreased with the increase of $CO_2$ flow rates. Modified $CO_2$ extractions with 10% methylene chloride showed a slight increase in the recoveries over pure $CO_2$ extraction. Quantity of fish tissues had great effect on their extraction efficiencies. Recoveries of OPPs were $66.7{\sim}86.3%$ for jacopever, $56.2{\sim}79.2%$ for yellow tail, $57.6{\sim}77.8%$ for blanquillo, $84.2{\sim}96.3%$ for sardine, $74.6{\sim}83.6%$ for mackerel. Application of supercritical carbon dioxide extraction offers an attractive alternative to the use of organic solvents for extraction of pesticide residues from fish tissues.

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