• Title/Summary/Keyword: extraction chromatography

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Development of Fast Screening Method for Crop Protection Agents in Tobacco by Stir Bar Sorptive Extraction and Thermal Desorption coupled to GC/MS

  • Min, Hye-Jeong;Lee, Jeong-Min;Shin, Han-Jae;Lee, Moon-Yong;Jang, Gi-Chul
    • Journal of the Korean Society of Tobacco Science
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    • v.36 no.1
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    • pp.26-33
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    • 2014
  • Simultaneous determination of crop protection agents(CPAs) in food are done with multi-residue methods, which are composed of sample clean-up, concentration, chromatographic separation and detection. Stir Bar Sorptive Extraction(SBSE) technique is used for sample preparation of various analytes in several fields. The aim of this study was to develop a sensitive and fast method based on SBSE followed by thermal desorption - gas chromatography - mass spectrometry(TD - GC/MS) to determine CPAs in tobacco sample. For the analysis of tobacco sample prior to the SBSE method, solvent extraction or ultrasound-assisted solvent extraction was performed. methanol was used as the extraction solvent. The extract was then diluted with water. Finally, the sample was subjected to SBSE. A method for fast screening of crop protection agents in tobacco using SBSE-TD - GC/MS has been developed. About 17 CPAs including organochlorine, organophosphorous and others were identified and quantified. This method showed good linearity and high sensitivity for most of the target CPAs. The method was applied to the determination of CPAs at ng/mL levels in tobacco sample. This method is simple, rapid and may be applied in detection of other components.

Comparisons of Volatile Compounds of Pinus densiflora on Kinds of Extraction Solvent and Parts of Pinus (솔 부위 및 추출 용매를 달리한 솔향의 분석)

  • 이양봉;조지은;이미정;윤정로
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.28 no.5
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    • pp.973-979
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    • 1999
  • Volatile compounds from twigs, needles and sprouts in Pinus densiflora were extracted with n hexane, diethyl ether or ethanol for 24 hours, and the extracted compounds were separated and identified by gas chromatography and mass selective detector. The kinds and amount of volatile compounds extracted from three parts of Pinus densiflora were different in solvent extraction and the extraction by the modified Liken Nickerson apparatus. The contents of volatile compounds of twigs contained more than those of needles and sprouts, and the volatile compounds were extracted more in n hexane than the others. In the extraction with hexane, the main volatile compounds of twigs were 18.5% pinene, 14.5% limonene, 12.7% pinene and 3.2% myrcene. Sprouts were 16.8% limonene, 4.4% pinene, 4.3% pinene and 1.7% myrcene. Needles contained 14.7% pinene, 5.4% pinene, 2.2% limonene and 0.8% myrcene. The highest yield for pine aroma was shown in the extraction from pine twigs with n hexane, and in this extraction the amounts of pinene, pinene and limonene were 742 g, 1108 g and 922 g per gram sample, respectively.

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Standardized microwave extract of Sappan Lignum exerts anti-inflammatory effects through inhibition of NF-κB activation via regulation of heme oxygenase-1 expression

  • Md Anisuzzaman Chowdhury;Moonbum Choi;Wonmin Ko;Hwan Lee;Sam Cheol Kim;Hyuncheol Oh;Eun‑Rhan Woo;Youn‑Chul Kim;Dong‑Sung Lee
    • Molecular Medicine Reports
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    • v.19 no.3
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    • pp.1809-1816
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    • 2019
  • The extract of Sappan Lignum, the heartwood of Caesalpinia sappan L., has been used in medicine to improve blood circulation. Recently, the application of microwave extraction methods has been a major focus of research into the extraction of components from natural sources. In this experiment, we compared the anti-inflammatory effects of Sappan Lignum prepared by heat-70% EtOH extraction (CSE-H-70E) and microwave-70% EtOH extraction (CSE-MW-70E). High-performance liquid chromatography analysis was used to identify the compounds in these extracts. The heat-70% EtOH and microwave-70% EtOH extracts of Sappan Lignum had different chromatograms. CSE-MW-70E significantly inhibited the protein expression of iNOS and COX-2, PGE2, TNF-α, and reduced NO and IL-1β production in macrophages exposed to LPS, whereas, only high concentrations of CSE-H-70E (20 ㎍/ml) resulted in any effects. Furthermore, CSE-MW-70E upregulated heme oxygenase-1 (HO-1) expression. In addition, the use of tin protoporphyrin, an inhibitor of HO-1, confirmed the inhibitory effects of CSE-MW-70E on pro-inflammatory mediators. These results suggested that the CSE-MW-70E-mediated upregulation of HO-1 played an important role in the anti-inflammatory effects of macrophages. Therefore, these findings showed that microwave extraction can be utilized to improve the extraction efficiency and biological activity of Sappan Lignum.

The Influence of Pressure and Time on the Preparation of Gumiganghwal-tang Decoctions

  • Kim, Jung-Hoon;Kim, Seong-Sil;Shin, Hyeun-Kyoo;Seo, Chang-Seob
    • The Journal of Korean Medicine
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    • v.34 no.4
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    • pp.12-20
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    • 2013
  • Objectives: This study compared Gumiganghwal-tang (GGT) decoctions produced using different pressure levels for various extraction times to determine the optimal extraction conditions through hydrogen ion concentration (pH), total soluble solids content (TSSC), extraction yield, and content of chemical compounds. Methods: Decoctions were prepared by the pressure levels of 0 or $1kgf/cm^2$ for 30-180 min. The pH and TSSC were measured, the extraction yield was calculated, and the amounts of the chemical compounds were determined using high performance liquid chromatography. Results: The higher pressure and longer extraction time decreased the pH value, while those conditions increased TSSC and extraction yield: the decoction produced in 180 min by pressurized method showed the minimum value of pH, but maximum values of TSSC and extraction yield. The chemical compounds showed higher amounts in decoctions produced by non-pressurized methods than pressurized methods and their amounts were decreased over the peak extraction time in both pressurized and non-pressurized methods. The results of regression analysis confirmed the correlative influences of the pressure and extraction time on pH, TSSC, and extraction yield. Conclusions: This study suggests that pressure and extraction time influence the compositional constituents in GGT decoctions, and the non-pressurized method for 120 min should be chosen as the optimal extraction condition for the preparation of GGT decoction.

Comparison of Extraction Methods for the Determination of Vitamin E in Some Grains (곡류 내 비타민 E 분석을 위한 추출방법의 비교)

  • Lee, Seon-Mi;Lee, Hee-Bong;Lee, Junsoo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.35 no.2
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    • pp.248-253
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    • 2006
  • For the determination of vitamin I using high performance liquid chromatography (HPLC), the most critical and time consuming step is the Quantitative extraction of all vitamin E homologs from sample matrix. Three different extraction methods were compared to determine vitamin E in grains. Saponification used alkaline hydrolysis followed by solvent extraction. Direct solvent extraction included dispersing the samples in hot water, addition of isopropanol and $MgSO_4$, and extraction of the analytes with extracting solvent with Polytron homogenization. Using Soxhlet extraction, the samples were extracted in a Soxhlet apparatus with hexane containing butylated hydroxytoluene (BHT). Vitamin E content in 14 grains were analyzed and compared by three different extraction methods. Generally, the highest values were observed from direct solvent extraction and Soxhlet extraction followed by saponification. a-Tocopherol equivalent (a-TE) levels in grains ranged from 0.32 a-TE/100 g in prosomillet to 5.12 a-TE/100 g in black rice.

Investigation of difference of Gwakhyangjeonggi-san decoctions produced by different pressure levels and various extraction times (전탕 압력과 전탕 시간의 차이에 따른 곽향정기산 전탕액 비교)

  • Kim, Jung-Hoon;Lee, Nari;Shin, Hyeun-Kyoo;Seo, Chang-Seob
    • Herbal Formula Science
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    • v.22 no.2
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    • pp.15-24
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    • 2014
  • Objectives : Gwakhyangjeonggi-san (GJS) which consists of 13 herbal medicines has been used to treat gastrointestinal disorders caused by common cold. This study was performed to compare GJS decoctions produced using different pressure levels for various extraction times. Methods : Decoctions were prepared by the pressure levels of $0kgf/cm^2$ (non-pressurized) or $1kgf/cm^2$ (pressurized) for 30-180 min. The extraction yield, total soluble solid content (TSSC), and hydrogen ion concentration (pH) were measured, and the contents of the nine marker compounds were determined using high performance liquid chromatography. Results : The higher pressure and longer extraction time significantly increased TSSC value, while decreased the pH value. However, only extraction time affected the extraction yield of pressurized decoction. Variation of the amounts of chemical compounds was shown in pressurized and non-pressurized decoctions during extraction time. The result of regression analysis showed that pressure and extraction time can influence to extraction yield, TSSC, pH, and the content of chemical compounds. Conclusions : This study suggests that the pressure and extraction time can significantly affect the extraction efficiency of components from GJS decoctions.

Assessment on the Extraction Efficiency of Explosive Compounds in Soil for Improving the Working Draft of International Standard (국제표준(안) 개선을 위한 토양 중 화약물질 추출 효율성 평가)

  • Lee, Goon-Taek;Jung, In-Ho;Kim, Bo-Hyun;Kim, Dong-Wook
    • Journal of Soil and Groundwater Environment
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    • v.17 no.1
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    • pp.42-46
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    • 2012
  • The ISO document of ISO/TC/190/SC3/WG11/N11 is a working draft of international standard (WD) dealing with analytical method for the determination of explosives and related compounds using high performance liquid chromatography. The scope of this WD covers the storage of samples, preparing test portion, extraction and instrumentation. The main purpose of this study was to improve the extraction conditions which were already adopted in the WD. For this purpose, mechanical shaking method could be corresponded up to 18 hours of ultrasonic bath extraction in the WD was tested. Methanol was also tested with the intention of being added as an extracting solvent other than acetonitrile in the WD. According to the results, 16 hours of mechanical shaking method showed statistically the same effectiveness as that of 18 hours of ultrasonic bath extraction. In case of extracting solvent, methanol also showed statistically the same extraction capability as acetonitrile for DNB, TNT, 2-A-DNT and 2,4-DNT. However, the recovery rate of TNB with methanol extraction was 40% higher than that of acetonitrile extraction. Through adding mechanical shaking method into committee draft (cf. the next stage draft of the WD during the process for making international standard), ISO standard of analyzing explosives and related compounds in soil would become more useful in dealing with huge number of field samples in the laboratory. In other aspect, adopting methanol as an alternative extracting solvent would be very effective in the terms of exchangeability with GC-ECD/MS method which is being developed by German experts.

The Structure and Antibiotic Activities of Hydroxy Acid of Lanostenol Compound in Daedalea dickinsii

  • Bae, Gang Gyu;Min, Tae Jin
    • Bulletin of the Korean Chemical Society
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    • v.21 no.12
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    • pp.1199-1201
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    • 2000
  • 31-Hydroxycarbowyacetylquercinic acid, a lanostenoid hydroxyl acid has been isolated from D. dickinsii by solbent extraction, silica gel column chromatography and recrystallization. The structure of this compound has been determined to be 31-hydroxycarboxyacetylquercinic acid by a combinationof spectral data and by HM-BC. This compound showed antimicrobial activities against human pathogenic fungi and bacteria.

Evaluation on Extraction Conditions and HPLC Analysis Method for Ginsenosides in Panax ginseng (인삼의 추출조건 및 진세노사이드의 HPLC 분석법 평가)

  • Lee, Kyeong Hee;Lee, Dae Young;Lee, Seung Eun;Nam, Ki Yeul;Hwang, Gwang Bo;Kim, Hyung Don;Lee, Jae Won;Choi, Je Hun;Ahn, Young Sup;Kim, Seung Yu;Kim, Geum Soog
    • Korean Journal of Medicinal Crop Science
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    • v.24 no.1
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    • pp.47-54
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    • 2016
  • Background : A new extraction method-heated ultrasonic extraction was qualitatively and quantitatively analyzed for the extraction of major ginsenosides from ginseng extract; this new high-performance liquid chromatography (HPLC) method was compared with the official extraction method of Korean industrial standards and standard for health functional food. Methods and Results : Ginsenoside compounds were analyzed for 35 minutes by the new HPLC analysis method using a Halo$^{(R)}$ RP-Amide column. The new HPLC analysis method was validated by the measurement of intra-day and inter-day precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of each ginsenoside. The correlation coefficients (r2) for the calibration curves of the ginsenoside compounds were over 0.9997 in terms of linearity. The heated ultrasonic extraction method using ultrasonication for 30 minutes at $50^{\circ}C$ yielded higher amount of ginsenosides than the extraction method of the Korean industrial standards owing to the enhancement of extraction efficiency. Conclusions : Compared to the other extraction methods, the heated ultrasonic extraction method yielded a higher amount of ginsenoside Rb1 than Rg1 index compounds for the quality evaluation of ginseng roots.

Compositional differences of Bojungikgi-tang decoctions using pressurized or non-pressurized extraction methods with variable extraction times

  • Kim, Jung-Hoon;Seo, Chang-Seob;Kim, Seong-Sil;Shin, Hyeun-Kyoo
    • The Korea Journal of Herbology
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    • v.28 no.4
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    • pp.1-6
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    • 2013
  • Objectives : In other to determine the optimal extraction conditions, the various Bojungikgi-tang (BJIGT) decoctions prepared by different pressure levels and different extraction times were compared and evaluated in terms of the extract yield and the total soluble solid content. Methods : Decoctions were prepared by the pressure levels of 0 (non-pressurized) and 1 $kgf/cm^2$ (pressurized) for 60, 120 and 180 min. The extract yield and the total soluble solids content of decoctions were measured, and the amounts of the reference compounds in decoctions were investigated by the analysis using high performance liquid chromatography. Results : The extract yield and the total soluble solid content were higher in decoctions extracted by the pressurized method than those from decoction with non-pressurized method. The patterns of yield and contents showed a proportional increase to the extraction time. In analysis of the linear regression for four reference compounds such as liquiritin, nodakenin, hesperidin, and glycyrrhizin, the good linearity with the correlation coefficient more than 0.9999 was observed. The highest contents for four reference compounds were observed at 180 min of both the pressurized method and the non-pressurized method. Conclusions : This study suggests that the pressure in extraction method and the extraction time affect the compositional constituents in BJIGT decoctions. The extraction time of 180 min could be chosen in both pressurized and non-pressurized method as optimal extraction condition.