• Title/Summary/Keyword: High performance Liquid Chromatography

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Comparison of Major Compounds in Illicii Veri Fructus by Extraction Solvents (추출용매에 따른 팔각회향의 주성분 함량비교)

  • Lee, A Yeong;Kim, Hyo Seon;Choi, Goya;Chun, Jin Mi;Moon, Byeong Cheol;Kim, Ho Kyoung
    • The Korea Journal of Herbology
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    • v.28 no.6
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    • pp.47-51
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    • 2013
  • Objectives : The Illicii Veri Fructus was not only traditional medicine but also food in Asia. The aim of this study was selection of optimum solvent in the fruit of Illicii Veri Fructus because an appropriate solvent affect a medicinal effect. Methods : Illicii Veri Fructus was carried out ultrasonic-assisted extraction as various solvents. Two main compounds, p-anisaldehyde and anethole, were successfully analyzed by high performance liquid chromatography-photodiode array detector (HPLC-PDA) and carried out method validation according to ICH guideline. The optimum solvent selected by comparing with yields of two main ingredients. Results : The p-anisaldehyde and anethole were detected at approximately 8.0 min and 19.8 min, respectively. It was all below 5.0% that RSD of retention time and peak area for two main peaks. Calibration curves of two compounds were good linearity as $R^2$ >0.9999. All of the precisions and accuracy were good intra-day and inter-day as below 5.0% RSD. Limited of detection (LOD) of p-anisaldehyde and anethole were analyzed as $0.134{\mu}g/mL$ and $4.286{\mu}g$, respectively. Limited of quantification (LOQ) of two compounds were $0.407{\mu}g$ and $12.989{\mu}g$, respectively. As a result of this study, p-anisladehyde was detected as 0.209 ~ 0.467%, however anethole was not detected in the distilled water. Conclusions : Anethole was main component as 5.329 ~ 6.815% except for water extraction. Methanol extraction among various solvents was detected the highest contents of p-anisaldehyde and anethole as 0.467(${\pm}0.008$)% and 6.815(${\pm}0.220$)%, respectively.

A Study on the Cleanliness Evaluation Methods for the Selection of Alternative Cleaning Agents (대체 세정제의 선정을 위한 세정성 평가방법 연구)

  • Shin, Jin-Ho;Lee, Jae-Hoon;Bae, Jae-Heum;Lee, Min-Jae;Hwang, In-Gook
    • Clean Technology
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    • v.15 no.2
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    • pp.81-90
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    • 2009
  • In this study various cleaning evaluation methods were tested and comparatively evaluated to help cleaning industry. In order to select alternative cleaning agents objectively and systematically, various cleaning evaluation methods such as gravimetric, optically simulated electron emission (OSEE), contact angle, and analytical instrument methods were employed for cleaning contaminants such as flux, solder and grease. The analytical instruments used in this work were Fourier transform infrared spectroscopy (FTIR), ultraviolet visible spectroscopy (UV-VIS) and high performance liquid chromatography (HPLC). The gravimetric method was able to measure cleaning efficiencies easily and simply, but it was not easy to analyze them precisely because of its limitation in the gravimetric measurement. However, the OSEE technique was able to measure quickly and precisely the clean ability of cleaning agents in comparison with the gravimetric method. The contact angle method was found to be necessary for taking special precaution in its application to the cleaning evaluation due to possible formation of tiny organic film on the substrate surface which might be generated from contaminants and cleaning agents. In case of precision analysis that cannot be done by gravimetric method, fine analytical instruments such as UV-VIS, FTIR and HPLC could be used in analyzing trace amount of flux, solder and grease quantitatively, which were extracted from the surface by special solvents.

Determining of polycyclic aromatic hydrocarbons in domestic vegetables and fruits (국내유통 채소류 및 과일류 중 다환방향족탄화수소 분석)

  • Hu, Soojung;Oh, Nam Su;Kim, Soo Yeon;Lee, Hyomin
    • Analytical Science and Technology
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    • v.19 no.5
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    • pp.415-421
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    • 2006
  • The following concentrations of some PAHs were investigated; [benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene, indeno (1,2,3-c,d)pyrene] in vegetables(n=160) and fruits(n=50). The food samples were purchased at the local markets in Seoul, Chuncheon, Daejeon, Kwangju and Pusan. The samples were radish, onion, bean sprouts, welsh onion, chinese cabbage, spinach, young pumpkin, garlic, cucumber, carrot, lettuce, sesame leaf, tangerine, persimmon, apple, pear and banana. The methodology involved ultrasonic extraction with dichloromethane, clean-up on Sep-Pak florisil cartridges and determination by HPLC/FLD (High Performance Liquid Chromatography/Fluorescence Detector). Overall method recoveries for 8 PAHs spiked into these products ranged from 95 to 102%. The mean level of the following PAHs were determined; benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene and indeno(1,2,3-c,d)pyrene in vegetables and fruits was N.D., 0.014 ng/g, 0.031 ng/g, 0.016 ng/g, 0.019 ng/g, 0.091 ng/g, 0.016 ng/g and N.D., respectively.

Rapid and simultaneous determination of metabolites of organic solvents in human urine by high-performance liquid chromatography using a monolithic column (Monolithic 칼럼을 이용한 뇨 중 유기용매 대사체의 신속한 HPLC 동시 분석)

  • Han, Sang Beom;Lee, Sang-Ju;Lee, Cheol-Woo;Yoon, Seo Hyun;Joung, Sun Kyung;Youm, Jeong-Rok
    • Analytical Science and Technology
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    • v.19 no.5
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    • pp.433-440
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    • 2006
  • A HPLC/UV method was developed and validated for the rapid and simultaneous determination of urinary metabolites of organic solvents, mandelic acid, hippuric acid, phenylglyoxylic acid, ortho-, meta- and para-methylhippuric acid, using a monolithic column. The mobile phase was composed of tetrabutylammonium bromide as ion-pairing reagent with a flow rate of 2.4 mL/min. The total run time was less than 2.5 min for all six analytes. Good linearities were obtained for all the metabolites with correlation coefficients above 0.9993. Intra-day precision, accuracy and inter-day precision was 0.01~7.32%, 83.9~116.3% and 0.01~7.16%, respectively. The method was validated and confirmed by quantification of the quality assurance samples of Industrial Safety and Health Research Institute, Korea Occupational Safety and Health Agency.

Determination of residual novobiocin in livestock products and fisheries products by HPLC (HPLC를 이용한 축·수산 식품 중 잔류 노보비오신의 분석)

  • Lee, Byung Kyu;Lee, Cheol-Woo;Lee, Sang-Ju;Jung, Eun Ha;Lim, Hyun Kyun;Han, Sang Beom
    • Analytical Science and Technology
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    • v.20 no.4
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    • pp.347-354
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    • 2007
  • A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in bovine, porcine, chicken, flatfish and japanese eel muscle has been developed and validated. The separation condition for HPLC/UV was optimized with phenyl hexyl ($4.6{\times}150mm$, $5{\mu}m$) column with 10 mM monobasic sodium phosphate buffer (pH 2.5)/acetonitrile (50/50, v/v) as the mobile phase at a flow rate of 1.0 mL/min and detection wavelength was set at 254 nm. Residues were extracted from tissue by blending with methanol and lipid materials were removed with n-hexane. Then, the methanol extract was evaporated to dryness under a nitrogen stream, reconstituted in the mobile phase. Aliquot of the organic extract was decanted and filtered through $0.45{\mu}m$ syringe filter. The $20{\mu}L$ of the resulting solution was injected into the HPLC system. The calibration ranges were $0.5{\sim}5{\mu}g/g$ and calibration curves were linear with coefficients of correlation better than 0.95. The limits of quantification were $0.5{\mu}g/g$ for all muscles. The recoveries of bovine, porcine, chicken, flatfish and japaneseel muscles were 99.8%, 102.4%, 91.0%, 104.0% and 93.0%, respectively. The procedures were validated according to the CODEX guideline, determining specificity, linearity, accuracy, precision, quantitation limit and recovery.

Bioequivalence of pioglitazone tablet to Actos® tablet (Pioglitazone 30 mg) (액토스정®(피오글리타존 30 mg)에 대한 염산피오글리타존정의 생물학적동등성)

  • Yeom, Hyesun;Lee, Tae Ho;Youm, Jeong-Rok;Song, Jin-Ho;Han, Sang Beom
    • Analytical Science and Technology
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    • v.22 no.1
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    • pp.101-108
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    • 2009
  • The bioequivalence of two pioglitazone tablets, Actos$^{(R)}$ tablet (Takeda Chemical Industries, reference drug) and Pioglitazone tablet (Boryung Company, test drug) was evaluated according to the guidelines of Korea Food and Drug Administration. Twenty-eight healthy male Korean volunteers received each medicine (pioglitazone dose of 30 mg) in a $2{\times}2$ crossover study with one week washout interval. After drug administration, blood samples were collected at specific time intervals from 0-36 hours. The plasma concentrations of pioglitazone were determined by high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The total chromatographic run time was 5 min and calibration curves were linear over the concentration range of 5-2000 ng/mL for pioglitazone. The method was validated for selectivity, sensitivity, linearity, accuracy and precision. The pharmacokinetic parameters were determined from the plasma concentration-time profiles of both formulations. The primary calculated pharmacokinetic parameters were compared statistically to evaluate bioequivalence between the two preparations. The 90% confidence intervals of the $AUC_t$ ratio and the $C_{max}$ ratio for Pioglitazone tablet and Actos$^{(R)}$ tablet were log0.9422~log1.1040 and log0.9200~log1.1556, respectively. Based on the statistical considerations, we can conclude that the test drug, Pioglitazone tablet was bioequivalent to the reference drug, Actos$^{(R)}$ tablet.

Levels of sulfonamides for animals in food (식품 중 설폰아마이드계 동물용의약품의 잔류실태)

  • Jeong, Jiyoon;Hong, Mooki;Choi, Dongmi
    • Analytical Science and Technology
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    • v.20 no.1
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    • pp.84-90
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    • 2007
  • To determine levels of 11 sulfonamides for animals in food, simultaneously, a selective method of high performance liquid chromatography with UV detector has been applied. The targets were sulfachlorpyridazine (SCP), sulfadiazine (SDZ), sulfadimethoxine (SDM), sulfisoxazole (SSX), sulfamerazine (SMZ), sulfamethazine (SMT), sulfamethoxazole (SMX), sulfamethoxypyridazine (SMP), sulfamonomethoxine (SMM), sulfaquinoxaline (SQX) and sulfathiazole (STZ). Food samples were beef, pork, chicken, milk and whole egg that were collected at the main 6 cities in Korea as Seoul, Busan, Daejon, Incheon, Mokpo and Gangneung. After homogenizing food samples with sodium phosphate solution and acetonitrile, it was extracted with n-hexane. The mobile phase gradient was a mixture of 5 mM potassium phosphate (pH 3.25) and methanol with a gradient ratio from 100:0 to 30:70. The UV wavelength was 270 nm. The overall recoveries were ranged from 75% to 95% and the limit of detection was minimum 0.004 mg/kg for SMT, and 0.007 mg/kg for STZ at signal/noise > 3, respectively. As results, sulfonamide drugs were not detected in most of the selected food samples, however, sulfamonomethoxine was detected in meat. The determined level of sulfamonomethoxine were 0.03 and 0.06 mg/kg for beef that were below the MRLs.

Qunatitative analysis of liquiritin and glycyrrhizin in glycyrrhizae radix by HPLC-MS/MS (HPLC-MS/MS에 의한 감초의 liquiritin과 glycyrrhizin의 분석)

  • Yu, Young-Beob;Kim, Mi-Jung;Huang, Dae Sun;Ha, Hye-Kyeong;Ma, Jin-Yeul;Shin, Hyeun-Kyoo
    • Analytical Science and Technology
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    • v.20 no.4
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    • pp.331-338
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    • 2007
  • Licorice, Glycyrrhizae Radix is widely used as a herbal medicines and a dietary supplements in East Asia. We employed high performance liquid chromatography electrospray ionization tandem mass spectrometry to determine liquiritin and glycyrrhizin in the Glycyrrhizae Radix. Liquiritin and glycyrrhizin in Glycyrrhizae Radix were ionized by positive ion pneumatically assisted electrospray and detected by HPLC-MS/MS in the multiple-reaction monitoring (MRM) mode using precursor ${\rightarrow}$ product ion combinations at m/z $436.2{\rightarrow}257.0$ and $823.4{\rightarrow}453.4$, respectively. The assay had a calibration range from 10 to 3,000 ng/mL. The limits of detection (LOD) of the liquiritin and glycyrrhizin were 0.4 ng/mL and 0.01 ng/mL, respectively. The reproducibility and repeatability (relative standard deviation) at different analyte concentrations varied from 103 to 113 % and 0.95 to 1.8 %, respectively. According to the above results, HPLC-MS/MS method permits assignment of tentative structures such as liquiritin and glycyrrhizin in the Glycyrrhizae Radix.

Neuroprotective effect of Coreopsis lanceolata extract against hydrogen-peroxide-induced oxidative stress in PC12 cells

  • Kyung Hye Seo;Hyung Don Kim;Jeong-Yong Park;Dong Hwi Kim;Seung-Eun Lee;Gwi Young Jang;Yun-Jeong Ji;Ji Yeon Lee
    • Korean Journal of Agricultural Science
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    • v.49 no.2
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    • pp.175-184
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    • 2022
  • The present study investigated the neuroprotective effects of Coreopsis lanceolate extract against hydrogen-peroxide (H2O2)-induced oxidative damage and cell death in pheochromocytoma 12 (PC12) cells. Reactive oxygen species (ROS), 2,2'-azinobis (3-ethylbebzothiazoloine-6-sulfonic acid) diammonium salt, and 1,1-diphenyl-2-picrrylhydrazyl radical scavenging activities, as well as the expression levels of proteins associated with oxidative damage and cell death were investigated. According to the results, C. lanceolate extract exhibited inhibitory activity against intracellular ROS generation and cell-damaging effects induced by hydroxyl radicals in a dose-dependent manner. Total phenolic and flavonoid contents were 22.3 mg·g-1 gallic acid equivalent and 16.2 mg·g-1 catechin equivalent, respectively. Additionally, a high-performance liquid chromatography (HPLC) assay based on the internal standard method used to detect phenolic compounds. The phenolic compounds identified in C. lanceolata extract contained (+)-catechin hydrate (5.0 ± 0.0 mg·g-1), ferulic acid (1.6 ± 0.0 mg·g-1), chlorogenic acid (1.5 ± 0.0 mg·g-1), caffeic acid (1.2 ± 0.0 mg·g-1), naringin (0.9 ± 0.0 mg·g-1), and p-coumaric acid (0.5 ± 0.0 mg·g-1). C. lanceolata extract attenuated pro-apoptotic Bax expression levels and enhanced the expression levels of anti-apoptotic Bcl-2, caspase-3, and caspase-9 proteins. Therefore, C. lanceolata is a potential source of materials with neuroprotective properties against neurodegenerative disorders, such as Alzheimer's and Parkinson's diseases.

Anti-inflammatory activities of carrot(Daucus carota) leaf Fermented by Weizmannia coagulans KK7 (김치에서 분리한 Weizmannia coagulans KK7으로 발효한 당근 잎 추출물의 함염증 활성 연구)

  • Yoonji Lee;Boram Ko;Hyejin Hyeon;Daeju Oh;Weon-Jong Yoon
    • Journal of the Korean Applied Science and Technology
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    • v.39 no.6
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    • pp.932-940
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    • 2022
  • In this study, the extracts of carrot (Daucus carota var. sativa) leaf fermented with Weizmannia coagulans KK7 strain were investigated for the anti-inflammatory activities and component changes. The KK7 strain was isolated from kimchi, a Korean fermented vegetable. The high-performance liquid chromatography was performed to analyze the changes in the components of the carrot leaf extracts before and after fermentation. It was confirmed that the content of luteolin, a kind of flavonoid, was significantly increased after fermentation. The anti-inflammatory activities of the carrot leaf extracts and the fermented carrot leaf extracts were evaluated by the inhibition of NO (nitric oxide) production in LPS-induced RAW 264.7 cells. The NO scavenging ability of the fermented carrot leaf extracts was higher than the other extracts. The protein expression of iNOS, an enzyme responsible for the NO production was significantly reduced in a concentration-dependent manner by treatment with the fermented carrot leaf extracts. In conclusion, we found that the anti-inflammatory effect of carrot leaf was increased by microbial fermentation, suggesting that carrot leaf generally discarded could be used as new food and cosmetic materials through fermentation.