• Title/Summary/Keyword: SPE1

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Preconcentration and Detection of Herbicides in Water by Using the On-line SPE-HPLC System and Photochemical Reaction

  • 이승호;이성광;박영훈;김현주;이대운
    • Bulletin of the Korean Chemical Society
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    • v.20 no.10
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    • pp.1165-1171
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    • 1999
  • The analysis of trace herbicides using the on-line SPE-HPLC system and a photochemical reaction was studied. 18 compounds of herbicides including eight triazines, six phenoxy acids and esters, and four other herbicides were examined. The on-line SPE-HPLC system developed for selection of eluting solvent improved chromatographic efficiency. The recoveries of herbicides were higher than 77%. With 100 mL tap water samples, the detection limits for all analytes were in the 0.1-2.3×10-10 M range. Detection was done by a UV or fluorescence spectrometer after photochemical reaction at the end of the column with 2W or 450W mercury lamp. Without a photochemical reaction, all compounds responded to 230 nm UV detector, but phenoxy acids and esters were weakly detected. However, with a photochemical reaction, these compounds were selectively detected at 320 nm wavelength of UV absorption and 400 nm emission of the fluorescence detectors. This method can be used for the analysis of environmental water containing herbicides at trace levels.

Rapid Identification of Bioactive Compounds Reducing the Production of Amyloid β-Peptide (Aβ) from South African Plants Using an Automated HPLC/SPE/HPLC Coupling System

  • Kwon, Hak-Cheol;Cha, Jin-Wook;Park, Jin-Soo;Chun, Yoon-Sun;Moodley, Nivan;Maharaj, Vinesh J.;Youn, Sung-Hee;Chung, Sung-Kwon;Yang, Hyun-Ok
    • Biomolecules & Therapeutics
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    • v.19 no.1
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    • pp.90-96
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    • 2011
  • Automated HPLC/SPE/HPLC coupling experiments using the Sepbox system allowed the rapid identification of four bioactive principles reducing the production of amyloid $\beta$-peptide ($A{\beta}$) from two South African plants, Euclea crispa subsp. crispa and Crinum macowanii. The structures of biologically active compounds isolated from the methanol extract of Euclea crispa subsp. crispa were assigned as 3-oxo-oleanolic acid (1) and natalenone (2) based on their NMR and MS data, while lycorine (3) and hamayne (4) were isolated from the dichloromethane-methanol (1:1) extract of Crinum macowanii. These compounds were shown to inhibit the production of $A{\beta}$ from HeLa cells stably expressing Swedish mutant form of amyloid precursor protein (APPsw).

Charge/discharge Characteristics of Polypyrrole/SPE/Li Cell with Polypyrrole film Prepared by Electropolymerization Method as a Function of Temperature (전해중합법에 의한 Polypyrrole/SPE/Li Cell의 온도에 따른 충방전 특성)

  • Kim, J.U.;Yu, Y.H.;Cho, J.C.;Jeong, W.J.;Park, G.C.;Park, B.K.;Gu, H.B.;Moon, S.I.
    • Proceedings of the KIEE Conference
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    • 1996.07c
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    • pp.1703-1706
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    • 1996
  • The purpose of this study is to research and develop polypyrrole(PPy) positive for thin film rechargeable lithium battery. We investigated cyclic voltammetry, AC impedance response and charge/discharge cycling of PPy/SPE/Li cells as a function of temperature. The redox capacity of $PPy/CF_{3}SO_{3}$ film was the most large. The discharge capacity of PPy/SPE/Li cell with $PPy/CF_{3}SO_{3}$ film was higher than those of $PPy/ClO_{4}$ and $PPy/AsF_6$ films at all cycles. The energy density of PPy/SPE/Li cells during 1st cycle was 73, 90 and 101Wh/kg at $25^{\circ}C$, $45^{\circ}C$ and $60^{\circ}C$, respectively. The improvement of energy density is due to reduction of charge-transfer resistance associated doping-undoping process in PPy film with Increasing temperature. $PPy/CF_{3}SO_{3}$ film shows a good property on charge/discharge cycling in PEO-$LiClO_4$-PC-EC electrolyte.

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Anti-obese related pharmacological effects of standard potato protein extracts on the 45%Kcal high fat diet supplied mice

  • Kang, Su-Jin;Song, Chang-Hyun;Kim, Jong-Kyu;Chun, Yoon-Seok;Han, Chang-Hyun;Lee, Young-Joon;Ku, Sae-Kwang
    • Journal of Society of Preventive Korean Medicine
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    • v.22 no.2
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    • pp.77-107
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    • 2018
  • Objectives : In present study, therefore, possible beneficial pharmacological activities of standard potato protein extracts (SPE) were observed on the mild diabetic obese mice. Methods : After end of 12 weeks of continuous oral administrations of three different dosages of SPE 400, 200 and 100 mg/kg, or metformin 250 mg/kg, analyzed the hepatoprotective, hypolipidemic, hypoglycemic, nephroprotective and anti-obesity effects, separately. In addition, liver antioxidant defense systems were additionally measured with lipid metabolism-related genes expressions and hepatic glucose-regulating enzyme activities for action mechanism. Results : All of diabetes and related complications including obesity were significantly inhibited by treatment of SPE 400, 200 and 100 mg/kg, dose-dependently, and they also dramatically normalized the hepatic lipid peroxidation and depletion of liver endogenous antioxidant defense system, the changes of the hepatic glucose-regulating enzyme activities, also changes of the lipid metabolism-related genes expressions including hepatic $AMPK{\alpha}1$ and $AMPK{\alpha}2$ mRNA expressions, dose-dependently. Especially, SPE 200 mg/kg constantly showed favorable inhibitory activities against type II diabetes and related complications as comparable to those of metformin 250 mg/kg in HFD mice, respectively. Conclusions : The present work demonstrated that SPE 400, 200 and 100 mg/kg showed favorable anti-diabetic and related complications including obesity refinement activities in HFD mice, through AMPK upregulation mediated hepatic glucose enzyme activity and lipid metabolism-related genes expression, antioxidant defense system and pancreatic lipid digestion enzyme modulatory activities.

In vitro screening of anti-skin aging and antioxidant properties of aqueous/solvent extracts from distinctive stages of silkworm (Bombyx mori L.) pupae

  • Rahul, Kamidi;Kweon, HaeYong;Kim, Hyun-Bok;Lee, Ji Hae
    • International Journal of Industrial Entomology and Biomaterials
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    • v.45 no.1
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    • pp.1-11
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    • 2022
  • Silkworm pupae, a by-product of the silk industry are known to be valuable resource of nutrients for humans as well as animals besides encompassing diverse bioactive constituents. However, there is a paucity of knowledge on their role in amelioration of oxidative stress and anti-skin aging properties. In the present study, we evaluated the inhibitory effect of aqueous as well as ethanolic (30% and 70%) extracts from distinct stages of male and female silkworm pupae belonging to two silkworm varieties on skin aging-related enzymes. The activities of collagenase, elastase and tyrosinase were effectively inhibited by 70% ethanolic silkworm pupal extracts (SPE), followed by 30% with aqueous extracts exhibiting meager inhibitory potential. SPE were also investigated for their antioxidant activity in oxidative-stressed murine fibroblasts (L929). The intracellular ROS and lipid peroxidation induced by tert-butyl hydroperoxide (t-BHP) in fibroblasts was better attenuated by pre treatment with ethanolic (30%) and aqueous extracts, respectively. The safety of the extracts was determined by studying their effect on fibroblast cell viability and it was found that none of the extracts were cytotoxic. Our findings indicate the potential utility of SPE as anti-aging components in cosmeceuticals.

Simultaneous Determination and Monitoring of Bisphenols in River Water using Gas Chromatography-Mass Spectrometry (GC-MS 를 이용한 하천수 중 Bisphenol계 화합물의 동시분석 및 모니터링)

  • Kim, Jihyun;Choi, Jeong-Heui;Kang, Tae-Woo;Kang, Taegu;Hwang, Soon-Hong;Shim, Jae-Han
    • Korean Journal of Environmental Agriculture
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    • v.36 no.3
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    • pp.154-160
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    • 2017
  • BACKGROUND:This study was carried out to establish an efficient sample preparation for the simultaneous determination of bisphenols (BPs) in river water samples using gas chromatography-mass spectrometry (GC-MS). Sample preparation was examined with conventional extraction methods, such as solid-phase extraction (SPE) and liquid-liquid extraction (LLE), and their efficiency was compared with validation results, including linearity of calibration curve, method detection limit (MDL), limit of quantification (LOQ), accuracy, and precision. METHODS AND RESULTS:The BPs (bisphenol A, BPA; bisphenol B, BPB; bisphenol C, BPC; bisphenol E, BPE; bisphenol F, BPF; bisphenol S, BPS) were analyzed using GC-MS. The range of MDLs by SPE and LLE methods was $0.0005{\sim}0.0234{\mu}g/L$ and $0.0037{\sim}0.2034{\mu}g/L$, and that of LOQs was $0.0015{\sim}0.0744{\mu}g/L$ and $0.0117{\sim}0.6477{\mu}g/L$, respectively. The calibration curve obtained from standard solution of $0.004{\sim}4.0{\mu}g/L$ (SPE) and $0.016{\sim}16{\mu}g/L$ (LLE) showed good linearity with $r^2$ value of 0.9969 over. Accuracy was 93.2~108% and 97.4~120%, and precision was 1.7~4.6% and 0.7~6.5%, respectively. The values of MDL and LOQ resulted from the SPE method were higher than those from the LLE method, particularly those values of BPA were highest among the BPs. Based on the results, the SPE method was applied to determine the BPs in river water samples. Water samples were collected from mainstream, tributary and sewage wastewater treatment plants (SWTPs) in the Yeongsan river basin. The concentration of BPB, BPC, BPE, BPF and BPS were not detected in all sites, whereas BPA was ranged $0.0095{\sim}0.2583{\mu}g/L$, which was $0.0166{\sim}0.0810{\mu}g/L$ for mainstreams, $0.0095{\sim}0.2583{\mu}g/L$ for tributaries, $0.0352{\sim}0.1217{\mu}g/L$ for SWTPs. CONCLUSION: From these results, the SPE method was very effective for the simultaneous determination of BPs in river water samples using GC-MS. We provided that it is a convenient, reliable and sensitive method enough to monitor and understand the fate of the BPs in aquatic ecosystems.

Mulberry Paper Bag μ-Solid Phase Extraction for the Analysis of Five Spice Flavors by Gas Chromatography-Mass Spectrometry

  • Yoon, Ok-Kyung;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.30 no.1
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    • pp.35-42
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    • 2009
  • Headspace micro solid phase extraction using mulberry paper bag (HS-MPB-$\mu$-SPE) has been developed and validated for the analysis of volatile flavor compounds from five spice by gas chromatography-mass spectrometry (GC/MS). HS-MPB-$\mu$-SPE was performed with adsorbent particles enclosed inside a mulberry paper bag. Four different kinds of adsorbents such as Tenax TA, Porapack Q, dimethylpolysiloxane and polyethylene glycol were tested. The extraction solvents compared were petroleum ether, methylene chloride, and chloroform. Better results were obtained when Tenax TA and petroleum ether were used. The limit of detection (LOD) and the limit of quantitation (LOQ) were in the range of 1.3 ng/mL and 4.3 ng/mL, respectively, for o-cymene as a model compound of monoterpene. Proposed method showed good reproducibility (3.3%, RSD) and good recoveries (94.0%). The HS-MPB- μ-SPE is very simple to use, inexpensive, rapid, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume (0.6 mL), there is minimal waste or exposure to toxic organic solvent and no further concentration step. This method allows successful characterization of the headspace in contact with the five spice sample. Strong trans-anethole from star anise or fennel is a characteristic flavor of five spice powders. HS-MPB-$\mu$-SPE combined with GC/MS can be a promising technique for the broad spectrum measurement of volatile aroma compounds from solid spices.

Simultaneous determination of amphetamine-like drugs in human urine by SPE and GC/MS (고체상추출과 GC/MS를 이용한 소변 중 암페타민계 마약성분 동시분석법)

  • Cheong, Jae Chul;Kim, Jin Young;In, Moon Kyo;Cheong, Won Jo
    • Analytical Science and Technology
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    • v.21 no.1
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    • pp.41-47
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    • 2008
  • Although liquid-liquid extraction (LLE) method has been used routinely for the analysis of amphetamine-like drugs (amphetamine; AP, methamphetamine; MA, 3,4-methylenedioxyamphetamine; MDA, 3,4-methylenedioxymethamphetamine; MDMA, 3,4-methylenedioxyethylamphetamine; MDEA), a solid-phase extraction (SPE) method, which can be automated, was applied for the simultaneous determination by GC/MS in human urine. Urine samples (3 mL) and 0.1 M phosphate buffer (1 mL, pH 7.0) were extracted by an automated SPE system. The eluent was evaporated, derivatized with trifluoroacetic anhydride (TFAA), and analyzed by GC/MS. The calibration curves was linear with correlation coefficient ($r^2$) above 0.994 in the ranges of 34.0 (AP), 28.0 (MDA)~1000.0 ng/mL for AP, MDA, and 50.0~2000.0 ng/mL for MA, MDMA, and MDEA. The limits of detection ranged from 4.0 to 10.0 ng/mL, and the limits of quantitation ranged from 12.0 to 34.0 ng/mL. The relative recoveries were 93.5~107.7 %. The precisions and accuracies were 1.9~14.8 % and -8.7~14.8 %, respectively. The present method was successfully applied to identify the MA or Ecstasy (MDMA) abusers in exact as well as rapid.

Solid Phase Extraction(SPE) of Curcuminoids from Turmeric by Optimization Analytical Condition (최적 분석조건에 의한 강황으로부터 Curcuminoids의 고체상추출(SPE))

  • Lee, Kwang Jin;Ma, Jin Yeul;Kim, Young Jun;Kim, Young Sik
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.13 no.10
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    • pp.4927-4935
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    • 2012
  • Turmeric is a medicinal herb with various pharmacological activities. Curcumin, demethoxycurcumin(DMC) and bisdemethoxycurcumin(BDMC) were extracted from turmeric by dipping and ultrasonic wave method. And extraction efficiency was identified using solid phase extraction(SPE). The extracted sample were simultaneously separated and analyzed from three kinds of commercial $C_{18}$ reversed-phase high performance liquid chromatography using water and acetonitrile as mobile phase with isocratic elution mode. Flow rate 1.0mL/min, injection volume $10{\mu}L$ and column oven temperature $40^{\circ}C$ at 425nm wavelength has been conducted. From the experimental results, the optimum mobile phase composition of water/acetonitrile 50/50vol% using RS tech column. It is evident that the amount of curcuminoids extracted(extraction time 4h) by 100% MeOH was higher than any aqueous MeOH composition. Finally, in 100% water extraction, the amount(mAU${\times}$mim) of curcuminoids extracted by SPE was 14.3 and 24.5 times respectively higher than ultrasonic wave and dipping method. The shown results can be applied as sources for pharmaceuticals and functional material.

The Electrochemical Properties of PAN-PVDF-PEGME Blend Polymer Electrolyte System (PAN-PVDF-PEGME Blend계 고분자전해질의 전기화학적 특성)

  • Ryu, Kwang Sun;Lee, Gye Joong;Liou, Kwang Kyoung;Kang, Seong Gu;Chang, Soon Ho
    • Journal of the Korean Chemical Society
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    • v.43 no.2
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    • pp.199-205
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    • 1999
  • The electrochemical properties of PAN-PVDF-PEGME blend polymer electrolyte system are investigated and the physical properties are also measured with varying the content of PEGME. This PEGME partially reduces the crystallinity of PVDF. The ionic conductivities of the polymer electrolytes are about $10^{-3}S/cm$, which may be applicable to a constituent of lithium secondary battery. From the temperature dependence of ionic conductivity, it is suggested that the ionic conductivity increases with the PEGME content due to the fomation of effective ion-conducting path. The cation transference number reaches its maximum value for the electrolytes (SPE 2) with 10 wt% PEGME and then decreases for further increase of PEGME contnet. The electrochemically stable range of SPE 1 (without PEGME) is about 4.3 V, but SPE 2-4 (PAN-PVDF-PEGME system) is about 4.6 V. When these polymer electrolyte are used as electrolyte in rechargeable battery and the cell performances are tested, the discharge capacity increses with the amount of PEGME. Therefore, PEGME increases the ionic conductivity, extends the electrochemical stable range, and finally improves the discharge capacity of cell adopting the electrolyte system.

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