• Title/Summary/Keyword: liquid recovery

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Determination of Formaldehyde in Cosmetics Using a Convenient DNPH Derivatization Procedure Followed by HPLC Analysis (간편한 DNPH 유도체화 HPLC 분석법을 이용한 화장품 중 포름알데하이드 분석)

  • Choi, Jongkeun
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.42 no.1
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    • pp.65-73
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    • 2016
  • Korea Food and Drug Administration (KFDA) has officially announced 2,4-dinitrophenylhydrazine (DNPH) derivatization - high performance liquid chromatography (HPLC) methods for analysis of formaldehyde. This study was conducted to develop a convenient derivatization method for cosmetics by improving complex pre-treatment procedures included in KFDA method. To simplify pre-treatment procedures of KFDA method, reaction conditions including pH, time and temperature were optimized. This pre-treatment method does not require complicate pre-treatment steps of KFDA method such as pH adjustment of test solution with acetate buffer (pH 5.0), solvent-solvent partitioning with dichloromethane and concentrating procedure with vacuum evaporator. Formaldehyde-dinitrophenylhydrazone (formaldehyde-DNP) product produced by derivatization reaction was separated and quantified with a reversed-phase HPLC, which was slightly modified with KFDA method. The linearity test showed good results with 0.9999 of correlation coefficient ($r^2$) in the range of 2 ~ 40 ppm of standard solutions. In this method, limit of detection (LOD) and limit of quantitation (LOQ) values for formaldehyde were 0.2 ppm and 0.5 ppm, respectively. In addition, recovery test demonstrated that the method was also accurate and reproducible. Therefore, the proposed method can be applicable to rapid analysis of formaldehyde in cosmetics.

Uranium Recovery from Nuclear Fuel Powder Conversion Plant Filtrate and its Thermal Decomposition Characteristics (핵연료분말 제조공정에서 발생된 여액으로부터 우라늄 회수 및 회수된 우라늄 화합물의 열분해 특성)

  • Jeong, Kyung-Chai;Jeong, Ji-Young;Kim, Byung-Ho;Kim, Tae-Joon;Choi, Jong-Hyeun
    • Journal of the Korean Ceramic Society
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    • v.39 no.2
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    • pp.204-209
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    • 2002
  • In this study, $UO_4{\cdot}2NH_4F$, the precipitates which has low solubility, was obtained by chemical precipitation method to recover and reuse the trace uranium from the liquid waste producing in AUC process and for this compound it was characterized by means of chemical analysis, TG-DTA, XRD and FT-IR analyses. This compound was analyzed as $UO_4{\cdot}2NH_4F$ and shape of this precipitate was hexagonal type, having the size of 2∼3 ${\mu}m$. Also, the intermediates were obtained as $UO_4F,\;UO_4,\;UO_3,\;and\;U_3O_8$ by the thermal decomposition over the temperature of 220, 310, 515 and 640$^{\circ}C$, respectively. It is concluded that under the condition of a constant heating rate of 5$^{\circ}C$/min in air atmosphere range of between room temperature and 800$^{\circ}C$, thermal decomposition reaction mechanism of $UO_4{\cdot}2NH_4F$ is as follow; $UO_4{\cdot}2NH_4F{\rightarrow}UO_4F{\rightarrow}UO_4{\rightarrow}UO_3{\rightarrow}U_3O_8$.

Simultaneous Determination of Hesperidin and Glycyrrhizin in Pyungwi-san by HPLC/DAD (HPLC-DAD를 이용한 평위산 중의 Hesperidin 및 Glycyrrhizin의 동시분석법 확립)

  • Lee, Mi-Kyeong;Choe, Ok-Gyeong;Park, Jin-Ho;Cho, Jung-Hee;Kim, Do-Hoon;Baek, Ju-Hyun;Kim, Hyo-Jin;Lee, Ki-Yong;Kim, Sang-Du;Kim, Young-Choong;Sung, Sang-Hyun
    • Korean Journal of Pharmacognosy
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    • v.39 no.3
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    • pp.199-202
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    • 2008
  • A high performance liquid chromatographic (HPLC) method for the simultaneous determination of hesperidin and glycyrrhizin was established for the quality control of traditional herbal medicinal preparation, Pyungwi-san (PWS). Separation and quantification were successfully achieved with a Waters XTerra RP18 column ($5{\mu}m$, 4.6 mm I.D. ${\times}$ 150 mm) by gradient elution of a mixture of acetonitrile and water containing 0.03% phosphoric acid (pH 2.03) at a flow rate of 1.0 ml/min. The diode-array UV/vis detector (DAD) was used for the detection and the wavelength for quantification was set at 230 nm. The presence of hesperidin and glycyrrhizin in this extract was ascertained by retention time, spiking with each authentic standard and UV spectrum. All four compounds showed good linearity $(r^2>0.995)$ in a relatively wide concentration ranges. The R.S.D. for intra-day and inter-day precision was less than 7.0% and the limits of detection (LOD) were less than 60 ng. The mean recovery of each compound was 99.0-105.6% with R.S.D. values less than 4.0%. This method was successfully applied to the determination of contents of hesperidin and glycyrrhizin in three commercial products of PWS. These results suggest that the developed HPLC method is simple, effective and could be readily utilized as a quality control method for commercial PWS products.

Soil Mechanical Properties for Fill Slope of Forest Road in Mt. Gari (춘천(春川) 가리산(加里山) 지역(地域)의 임도(林道) 성토사면(盛土斜面)의 토질역학적(土質力學的) 특성(特性))

  • Cha, Du Song;Chun, Kun Woo;Ji, Byoung Yun;Oh, Jae Heun
    • Journal of Forest and Environmental Science
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    • v.15 no.1
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    • pp.98-106
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    • 1999
  • This study was carried out to analyze the mechanical properties of soil for counterplan of recovery construction and the slope stability on fill slope of Sang-gul forest road in Mt. Gari. To analyze the mechanical properties of apparent soil on fill slope in forest road, various soils such as soil, gravelly sandy soil, weathered rock were used as experimental sample in this study. In each experimental sample, particle size distribution test, liquid limit test, plastic limit test, and specific gravity test were carried by Korean industrial standards(KS F 2302, KS F 2303, KS F 2304, KS F 2306, KS F 2308). Through the results of soil particle size distribution analysis, soil moisture content analysis, and specific gravity analysis, soil texture, uniformity coefficient, curvature coefficient, dry density and specific gravity were able to be determined in sampling site. As a results in this study, soil was classified as SP, SW, GP by Unified Soil Classification Standard (USCS). specific gravity and dry unit weight of soil have the value range of 2.52~2.60 and 1.39~1.43, respectively. Also plastic index showed non plastic condition.

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Residues of Thiamphenicol in Blood of Cultured Olive Flounder and Black Rockfish Treated by Single Oral Administration (Thiamphenicol의 단일 경구투여에 따른 넙치와 조피볼락의 혈액내 잔류 분석)

  • JUNG, Sung-Hee;SEO, Jung-Soo
    • Journal of Fisheries and Marine Sciences Education
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    • v.28 no.3
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    • pp.692-700
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    • 2016
  • This study was aimed at investigating the residual patterns of thiamphenicol (TP) in the cultured olive flounder (Paralichthys olivaceus) and black rockfish (Sebastes schlegeli) following oral administration. TP concentration were detected by high performance liquid chromatography with UV detector. The recovery rates of TP in serums ranged 77.05~97.23% (olive flounder) and 89.96~97.11% (black rockfish) for the concentration of 0.1, 1.0, $10{\mu}g/mL$, respectively. After single administration of TP (100 mg/kg body weight) by oral route in olive flounder ($700{\pm}50g$, $23{\pm}1.5^{\circ}C$) and black rockfish ($500{\pm}30g$, $23{\pm}1.5^{\circ}C$), the concentration in the serum was determined at 1, 5, 10, 15, 24, 30, 50, 168, 264 and 432 h post-dose. Two-compartment model was applied to analyze in the pharmacokinetics of TP administered to the fishes. In the serum of olive flounder, TP was detected on 10 and 15 hours after treatment were $10.08{\mu}g/mL$ and $10.06{\mu}g/mL$ as maximum level, respectively. In the serum of black rockfish, TP was detected on 15 hours after treatment were $8.88{\mu}g/mL$ as maximum level. Concentrations of TP to the fishes were not measurable at 432 hours (18 days) after treatment in all samples. Similar residual patterns of TP were revealed between the fishes. These results are helpful for estimating withdrawal time of TP which has been already in use for farmed fish treatment.

Evaluation of Tar Dyes Used in Commercial Foods (식품 중 합성첨가물 사용실태 조사 연구 -타르색소 중심으로-)

  • 윤미혜;김국주;김정임;황선일;문수경;정은주;김재관
    • Journal of Food Hygiene and Safety
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    • v.15 no.2
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    • pp.108-113
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    • 2000
  • This study was carried out to propose a simple method for the extraction of seven tar dyes such as tartrazine, sunset yellow FCF, amaranth, erythrosine, allura red, brilliant blue FCF and indigo carmine using aminopropyl amine cartridge and to determine the content of the dyes in candies, soft drinks, ice bars and okchuns produced in Korea. The tar dyes were simultaneously analyzed by reverse phase high performance liquid chromatography(HPLC). The recovery rates of the dyes ranged from 65.8% to 99.6%. The contents of the dyes in candies, soft drinks, ice bars and octhuns were N.D.∼50.1 mg/kg, N.D.∼49.9 mg/kg, N.D.∼56.0 mg/kg and N.D.∼867.3 mg/kg, respectively. The types of the dyes used most frequently for candies, soft drinks and ice bars were tartrazine, brilliant blue and amaranth, respectively. Of the samples, tartrazine was used frequently, and indigo carmine was not used at all.

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Residues of Ampicillin and Amoxicillin in Olive Flounder Paralichthys olivaceus Following Oral Administration (양식 넙치(Paralichthys olivaceus)에 경구투여한 Ampicillin 및 Amoxicillin의 어류체내 잔류량의 변화)

  • Son, Kwang-Tae;Jo, Mi-Ra;Oh, Eun-Gyoung;Mok, Jong-Soo;Kwon, Ji-Young;Lee, Tae-Seek;Song, Ki-Cheol;Kim, Poong-Ho;Lee, Hee-Jung
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.44 no.5
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    • pp.464-469
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    • 2011
  • Residues of ampicillin and amoxicillin in the muscles of olive flounder Paralichthys olivaceus were investigated after oral doses of 20 mg/kg body weight/day of ampicillin and 40 mg/kg body weight/day of amoxicillin in a first examination and 40 mg/kg body weight/day of ampicillin and 80 mg/kg body weight/day of amoxicillin in a second examination for 5-6 days. The ranges of seawater temperatures in the $1^{st}$ and $2^{nd}$ examinations were $13.4-15.6^{\circ}C$ and $16.8-21.4^{\circ}C$, respectively. Ampicillin and amoxicillin concentrations were analyzed by high performance liquid chromatography (HPLC). The average recovery rates of ampicillin and amoxicillin in fish samples ranged from 84.8-95.2% and 100.8-103.8%, respectively. Residual concentrations in the olive flounder peaked on the $5^{th}$ day, with average concentrations of 0.075 mg/kg and 0.311 mg/kg in the $1^{st}$ examination, and 0.098 mg/kg and 0.630 mg/kg in the $2^{nd}$ examination for ampicillin and amoxicillin, respectively, with maximum concentrations in muscle. In the $1^{st}$ examination, ampicillin concentrations in olive flounder after withdrawals of 1 and 3 days were 0.041 mg/kg and 0.023 mg/kg, respectively, and amoxicillin concentrations after withdrawals of 1 day and 10 days were 0.172 mg/kg and 0.023 mg/kg, respectively. In the $2^{nd}$ examination, the ampicillin concentrations in olive flounder after withdrawals of 1 and 3 days were 0.041 mg/kg and 0.023 mg/kg, respectively, and amoxicillin concentration after withdrawals of 1 day and 10 days were 0.172 mg/kg and 0.023 mg/kg, respectively. We suggest that the recommended withdrawal periods should be 3 days for ampicillin and 10 days for amoxicillin in the olive flounder.

Residues of Fluoroquinolones in Olive Flounder (Paralichthys olivaceus) and Black Rockfish (Sebastes schlegell) Following Oral Administration (Fluoroquinolone계 항생제의 경구투여에 따른 양식넙치 및 조피볼락의 체내 잔류량의 변화)

  • Kim, Poog-Ho;Lee, Doo-Seog;Kim, Jin-Woo;Park, Mi-Seon;Kim, Dong-Soo;Jo, Mi-Ra
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.42 no.4
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    • pp.329-334
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    • 2009
  • The residues of fluoroquinolones in Olive flounder (Paralichthys olivaceus) and Black rockfish (Sebastes schlegeli) were investigated after oral doses of 20 mg/kg for 30 days. Blood samples were taken at 5 hours, 10 hours, 1 day, 2 days, 3 days, 5 days, 7 days, 9 days, 13 days, 20 days and 30 days after treatment. The concentrations of fluoroquinolones were detected by high performance liquid chromatography using a UV detector. The recovery rates of fluoroquinolones in fish samples ranged from 92.0-99.7%, 93.4-97.5% and 93.0-97.9% for treatment of 0.1, 0.5, and $1.0{\mu}g/g$, respectively. Ciprofloxacin, enrofloxacin, norfloxacin and sarafloxacin were detected in the blood of the olive flounder at 10 hours, 10 hours, 1 day and 10 hours after treatment with $6.43{\mu}g/g$, $6.07{\mu}g/g$, $11.83{\mu}g/g$ and $11.02{\mu}g/g$ as maximum level, respectively. Ciprofloxacin, enrofloxacin, norfloxacin and sarafloxacin were detected in the blood of black rockfish 1 day, 1 day, 1 day and 10 hours after treatment with $8.26{\mu}g/g$, $8.03{\mu}g/g$, $7.29{\mu}g/g$ and $9.38{\mu}g/g$ as maximum level, respectively. However, ciprofloxacin, enrofloxacin, norfloxacin and sarafloxacin were not detected in olive flounder samples at 20, 30, 20 and 20 days after treatment in any experiments (

Effect of Cooking Methods on S-Allyl-L-Cysteine Content of Garlic (마늘의 조리방법에 따른 S-Allyl-L-Cysteine 함량 변화)

  • Lee, Sang Hoon;Jeong, Yun Sook;Hwang, Kyung-A;Song, Jin;Noh, Geon Min;Hwang, In Guk
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.8
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    • pp.1221-1226
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    • 2016
  • This study investigated changes in the S-allyl-L-cysteine (SAC) content of garlic using different cooking methods. Methods for determining SAC were validated by determining specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy using an high-performance liquid chromatography-fluorescence detection system. Results showed high linearity in the calibration curve with a coefficient of correlation ($R^2$) of 0.9999. The LOD and LOQ values for SAC were 0.15 and $0.47{\mu}g/mL$, respectively. The relative standard deviations for intra- and inter-day precision of SAC were less than 5%. The recovery rate of SAC was in the range from 97.35% to 97.47%. The SAC content of raw garlic was 2.77 mg/g, and there was no significant difference in SAC content according to blanching and microwave treatment. However, SAC content upon boiling and autoclaving at $110^{\circ}C$ and $121^{\circ}C$ increased from 3.50~9.16 mg/g, 6.52~16.21 mg/g, and 14.15~50.24 mg/g with increasing cooking temperature and time, respectively.

Simultaneous determination of baicalin and glycyrrhizin in Sosiho-tang by HPLC and anti-inflammatory activity (소시호탕에서 baicalin과 glycyrrhizin 동시 분석 및 항염 활성)

  • Kim, Jung-Hoon;Ha, Hye-Kyung;Seo, Chang-Seob;Lee, Jin-Ah;Shin, Hyeun-Kyoo
    • The Korea Journal of Herbology
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    • v.26 no.1
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    • pp.41-46
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    • 2011
  • Objectives : To quantitate the main compounds and investigate the biological activity of Sosiho-tang (Xiao-Chai-Hu-Tang, SST), simultaneous determination of baicalin and glycyrrhizin, and anti-inflammatory activity were estimated. Methods : A quantitative analysis was performed using a high performance liquid chromatography (HPLC). Reference compounds were separated on a reversed-phase column using gradient elution with water and acetonitrile each containing acetic acid at a flow rate of 1 mL/min. And the productions of nitric oxide (NO) and prostaglandin $(PE)E_2$ were examined by lipopolysaccharide (LPS)-treated RAW 264.7 cells in the presence of the SST. The anti-inflammatory activity of SST was investigated by carrageenin-induced paw edema in rats. The paw volume was measured at 2 and 4 hr following carrageenin-induced paw edema in rats. Results : The correlation coefficients of the compounds showed good linearity ($r^2$ > 0.9992) over the linear range. The precisions of intra- and inter-day were less than 7.0% of relative standard deviation (RSD) values for baicalin and less than 3.5% of RDS valuse for glycyrrhizin. Recovery rates were within the range of 95.41-101.5%. The contents of baicalin and glycyrrhizin in SST were average 70.52, 6.18 mg/g, respectively. And SST exhibited inhibitory effect on NO production in LPS-treated RAW 264.7 cells but not on $PGE_2$ production. Oral administration of SST (1 g/kg) showed a reduction in carrageenin-induced paw edema on rats. Conclusions : The analytical method was applied successfully to measure the contents of baicalin and glycyrrhizin in SST which exhibited anti-inflammatory activities.