• Title/Summary/Keyword: soxhlet extraction

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Study on analysis of PAHs in consumer products (공산품 함유 PAHs 분석법에 관한 연구)

  • Song, Moon Hwan;Cho, Young Dal;Choe, Eun Kyung
    • Analytical Science and Technology
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    • v.27 no.4
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    • pp.201-212
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    • 2014
  • Polycyclic aromatic hydrocarbons (PAHs) that are carcinogenic and persistent will be restricted in consumer products from December 27, 2015 by EU REACH regulation. Pretreatment using Soxhlet extraction and quantitative analysis by GC-MS were studied to develop the method for analyzing 18 PAHs in consumer products as well as to detect the amounts and the kinds of PAHs in consumer products such as grips of a bag and a hammer, a cable and a plastic sandal. Linearity and precisions were evaluated by analyses of the standard PAH solutions ranging from 0.3125 mg/L to 5.00 mg of each of 18 PAHs. Linearity of resulting standard curves for all 18 PAHs were obtained with $R^2$ above 0.999. Precisions of the retention times and the peak areas were found to be 0.00%~0.05% and 1.16%~3.69% of relative standard deviations, respectively. The recoveries for spiked samples were all around 95%~105% after Soxhlet extration using three different solvents such as dichloromethane, hexane and toluene. The limits of quantitation for 18 PAHs in solutions and polymer samples by GC-MS were evaluated to be 0.327 mg/L (Benzo[ghi]perylene)~0.464 mg/L (Acenaphthylene) and 1.635 mg/kg (Benzo[ghi]perylene)~2.32 mg/kg (Acenaphthylene) based upon dilution factor of 5, respectively. Under the developed analytical method, only trace amounts of phenanthrene were detected in three samples while 15 kinds of PAHs including phenanthrene were detected in a grip of hammer with concentrations of maximum 83.4 mg/kg of Phenanthrene and minimum 8.5 mg/kg of Acenaphthylene. Further studies are needed to decrease the quantitation limit and to check the feasibility of decreasing Soxhlet time as well as to demonstrate cases that the clean up is required.

Primary study of sterols composition of Rhodiola sachalinensis by using GC/MS (GC/MS를 이용한 고산 홍경천의 스테롤 구성에 대한 초기연구)

  • Jin, Yinzhe;Li, Xifeng;Li, Donghao;Row, Kyung Ho
    • Analytical Science and Technology
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    • v.22 no.3
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    • pp.219-227
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    • 2009
  • The steroid compounds in Rhodiola sachalinensis were determined with adsorption column chromatographic purification and GC/MS. Sterols were extracted by sonication and Soxhlet with ethanol and dichloromethane, respectively. The extract was partitioned with chloroform and water using liquid-liquid extraction, and purified with a silica column after the sterols had been converted to the corresponding silyl derivatives with BSTFA. Eighteen free sterols, including $\beta$-sitosterol, stigmasterol and cycloartenol, and nine sterol conjugates were found from Rhodiola sachalinensis by GC/MS. Among them, cholest-5-ene-3-ol, cholesterol, stigmasterol, $\beta$-sitosterol were confirmed and quantified with sterol standards. Most sterols were presented in the chloroform part, with $C_{29}$ being the most abundant group in this sterol group. $\beta$-sitosterol was the most abundant compound with a relative content of 45.94% followed by ergost-7-ene-3-ol (11.33%), 4,14-dimethyl-ergosta-8,24(28)-diene-3-ol (7.07%), stigmasterol (6.09%), cycloartenol (5.43%) and 4-methyl-cholest-5-ene-3-ol (5.39%).

Phytochemical analysis of Panax species: a review

  • Yang, Yuangui;Ju, Zhengcai;Yang, Yingbo;Zhang, Yanhai;Yang, Li;Wang, Zhengtao
    • Journal of Ginseng Research
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    • v.45 no.1
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    • pp.1-21
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    • 2021
  • Panax species have gained numerous attentions because of their various biological effects on cardiovascular, kidney, reproductive diseases known for a long time. Recently, advanced analytical methods including thin layer chromatography, high-performance thin layer chromatography, gas chromatography, high-performance liquid chromatography, ultra-high performance liquid chromatography with tandem ultraviolet, diode array detector, evaporative light scattering detector, and mass detector, two-dimensional high-performance liquid chromatography, high speed counter-current chromatography, high speed centrifugal partition chromatography, micellar electrokinetic chromatography, high-performance anion-exchange chromatography, ambient ionization mass spectrometry, molecularly imprinted polymer, enzyme immunoassay, 1H-NMR, and infrared spectroscopy have been used to identify and evaluate chemical constituents in Panax species. Moreover, Soxhlet extraction, heat reflux extraction, ultrasonic extraction, solid phase extraction, microwave-assisted extraction, pressurized liquid extraction, enzyme-assisted extraction, acceleration solvent extraction, matrix solid phase dispersion extraction, and pulsed electric field are discussed. In this review, a total of 219 articles published from 1980 to 2018 are investigated. Panax species including P. notoginseng, P. quinquefolius, sand P. ginseng in the raw and processed forms from different parts, geographical origins, and growing times are studied. Furthermore, the potential biomarkers are screened through the previous articles. It is expected that the review can provide a fundamental for further studies.

Sorption of ο-Cresol by Granular Activated Carbon (GAC) and Abiotic Transformation on GAC Surface (입상활성탄에 의한 오르토크레졸(ο-cresol)의 흡착과 비생물학적 변형)

  • 한인섭;김용환
    • Journal of Soil and Groundwater Environment
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    • v.9 no.1
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    • pp.87-94
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    • 2004
  • The effects of pretreatment of GAC and dissolved oxygen (DO) on the sorption capacity for ο-cresol were investigated using pretreated GAC under oxic and anoxic conditions. Virgin GAC was used with pretreated GACs by $O_2$, acid and base as sorbents. Sorption capacity of GAC was dependent on the oxygen conditions according to the pretreatment methods. Virgin GAC showed increased sorption capacity when DO was present in the solution, while $O_2$-pretreated GAC did not show any considerable capacity change. Acid- and base-pretreated GACs were relatively more influenced by presence of DO as compared with virgin GAC. Both acid and base-pretreated GACs showed a rapid sorption rate at the initial stage, but as contact time became longer the sorption was slower. Sorbed ο-cresol was extracted with micro-Soxhlet extraction apparatus using the GAC separated from the rate experiments. Within 1 hour both acid and base-pretreated GACs showed the decrease in extraction efficiencies under both oxic and anoxic conditions. After 1 hour such a trend (the increase as contact time was longer) was not observed and showed relatively constant efficiencies of 35∼50%. According to the results of this study $O_2$contacted with GAC before sorption as well as DO present in the solution during sorption could influence the GAC sorption capacity.

Fundamental study on the development of the testing method of Triclosan with GC/ECD and GC/MS (GC/ECD 및 GC/MS를 이용한 트리클로산 정량분석에 관한 기초 연구)

  • Jeong, Hui-Jae;Lee, Jae-In;Kweon, Deok-Jun;Eom, Hui-Jeong;Choi, Zel-Ho;Choi, Ki-In
    • Analytical Science and Technology
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    • v.25 no.6
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    • pp.410-415
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    • 2012
  • In this study, a fundamental study was conducted to establish the method for quantitative analysis and pretreatment of triclosan, one of the chemicals to be used as bactericides, detergents, and sterilizers. The extraction efficiency of triclosan was the highest when it was extracted by soxhlet apparatus with n-hexane, and it showed a satisfactory result when the samples were analyzed with both GC/ECD and GC/MS. To evaluate the reproductivity of the results, each 30 reference samples made with paper filter and cotton wool was prepared in this study. From the results with high extraction effectiveness, low analysis deviation, and good statistical analysis data, the method for the extraction and analysis for triclosan were resonable for the paper and textile samples applied in this study.

A study of analytical method for Benzo[a]pyrene in edible oils (식용유지 중 벤조피렌 분석법 비교 연구)

  • Min-Jeong Kim;jun-Young Park;Min-Ju Kim;Eun-Young Jo;Mi-Young Park;Nan-Sook Han;Sook-Nam Hwang
    • Analytical Science and Technology
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    • v.36 no.6
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    • pp.291-299
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    • 2023
  • The benzo[a]pyrene in edible oils is extracted using methods such as Liquid-liquid, soxhlet and ultrasound-assisted extraction. However these extraction methods have significant drawbacks, such as long extraction time and large amount of solvent usage. To overcome these drawbacks, this study attempted to improve the current complex benzo[a]pyrene analysis method by applying the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method that can be analyzed in a simple and short time. The QuEChERS method applied in this study includes extraction of benzo[a]pyrene into n-hexane saturated acetonitrile and n-hexane. After extraction and distribution using magnesium sulfate and sodium chloride, benzo[a]pyrene is analyzed by liquid chromatography with fluorescence detector (LC/FLR). As a result of method validation of the new method, the limit of detection (LOD) and quantification (LOQ) were 0.02 ㎍/kg and 0.05 ㎍/kg, respectively. The calibration curves were constructed using five levels (0.1~10 ㎍/kg) and coefficient (R2) was above 0.99. Mean recovery ratio was ranged from 74.5 to 79.3 % with a relative standard deviation (RSD) between 0.52 to 1.58 %. The accuracy and precision were 72.6~79.4 % and 0.14~7.20 %, respectively. All results satisfied the criteria ranges requested in the Food Safety Evaluation Department guidelines (2016) and AOAC official method of analysis (2023). Therefore, the analysis method presented in this study was a relatively simple pretreatment method compared to the existing analysis method, which reduced the analysis time and solvent use to 92 % and 96 %, respectively.

Analyses of Additives Applied in a Polycarbonate (폴리카보네이트에 사용된 첨가제의 분석)

  • Kim, Seog-Jun
    • Analytical Science and Technology
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    • v.13 no.3
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    • pp.282-290
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    • 2000
  • In this study, polymer additives were extracted and separated by Soxhlet extraction method and the dissolution-precipitation method from a polycarbonate (optical grade) which completely absorbed UV light below 390 nm. Analytical techniques such as UV-Vis spectroscopy, FT-IR, and HPLC were applied to analyze additives in polycarbonate. Separated materials from the polycarbonate may be a complex mixture containing additives such as UV stabilizer, antioxidants (primary and secondary), monomers, and oligomers. Several compounds such as bisphenol A, Irganox 1010, and Cyasorb UV-5411 were identified by chromatograms and UV spectra obtained from RP HPLC analysis using Bondapak $C_{18}$ column, methanol mobile phase, and a photodiode array (PDA) detector. Also, the content of UV-5411 in the polycarbonate was about 0.12 wt% by a quantitative analysis through UV spectroscopy.

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Study on the Flavour of Garlic Extract (마늘 추출물의 향기성분에 관한 연구)

  • Park, Chul-Jin;Kim, Sang-Duk;Oh, Sung-Ki
    • Korean Journal of Food Science and Technology
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    • v.25 no.6
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    • pp.593-595
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    • 1993
  • The volatile components of garlic extracts were investigated. For experiment both crushed- and sliced-garlic were dried by air-drying and freeze-drying methods, followed by ether extraction. The extracts were analysed by GC and GC/MS. Sliced- and freeze-dried garlic extracts showed larger number of volatile components than crushed- and air-dried garlic extracts. The volatile components, allyl propyl disulifde, 2-vinyl-1,3-dithiane, 3-vinyl-〔4H〕-1,2-dithiin, 1,2-Bis (allyl)disulfane were found in sliced- and freeze-dried garlic extracts, methyl allyl trisulfide and 2,4-methyl furane in sliced- and air-dried garlic extracts, and disulfide in crushed- and air-dried garlic extracts.

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Hypoglycemic Activity of Ficus racemosa L. (Moraceae) Leaves in Streptozotocin-induced Diabetic Rats

  • Mandal, Subhash C.;Mukherjee, Pulok K.;Saha, Kakali;Das, J.;Pal, M.;Saha, B.P.
    • Natural Product Sciences
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    • v.3 no.1
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    • pp.38-41
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    • 1997
  • The hypoglycemic effect of the extract of Ficus racemosa leaves was studied on streptozotocin-induced diabetic rats. Petroleum ether $(60-80^{\circ}C)$ extract of the plant obtained by soxhlet extraction from coarsely pulverised leaves was used. In the $LD_{50}$ determination of the extract no abnormalities were observed at the dose range of 3 g/kg (p.o.) of the extract. The extract (200 mg/kg and 400 mg/kg orally) caused a reduction of blood glucose levels in streptozotocin-induced diabetic rats by 28.9% (P<0.00l) and 34.6% (P<0.001) respectively at the end of 9 days. The results. of this study indicate that the petroleum ether $(60-80^{\circ}C)$ extract of the leaves possesses significant hypoglycemic activity in hyperglycemic animals compared with glybenclamide as standard drug.

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Preparation of Molecularly Imprinted Polymers Using Photocross-linkable Polyphosphazene and Selective Rebinding of Amino Acids

  • Lee, Seung-Cheol;Chang, Ji-Young
    • Macromolecular Research
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    • v.17 no.7
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    • pp.522-527
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    • 2009
  • A photocrosslinkable polyphosphazene was used for molecular imprinting. We synthesized polyphosphazene (3) having urea groups for complexation with N-carbobenzyloxyglycin (Z-Gly-OH, template) and chalcone groups for cross-linking reaction. As substituents, 4-hydroxycha1cone (1) and N-(4-hydroxyphenyl)-N'-ethylurea (2) were prepared. Choloro groups of poly(dichlorophosphazene) were replaced by the sequential treatment with sodium salts of compounds 1 and 2, and trifluoroethanol. The template molecule was complexed with the urea groups on the polymer chains via hydrogen bonding. A thin polymer film was prepared by casting a solution of the complex of polymer 3 and the template in dimethylformamide on a quartz cell and irradiated with 365 nm UV light to yield a cross-linked film with a thickness of about $16{\mu}m$. The template molecules in the film were removed by Soxhlet extraction with methanol/acetic acid. The control polymer film was prepared in the same manner for the preparation of the imprinted polymer film, except that the template and triethylamine were omitted. In the rebinding test, the imprinted film exhibited much higher recognition ability for the template than the control polymer. We also investigated the specific recognition ability of the imprinted polymer for the template and its structural analogues. The rebinding tests were conducted using Z-Glu-OH, Z-Asp($O^tBu$)-OH, and Z-Glu-OMe. The imprinted film showed higher specific recognition ability for the template and the lowest response for Z-Asp($O^tBu$)-OH.