• Journal of the Korean GEO-environmental Society
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• v.11 no.5
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• pp.61-67
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• 2010

In this study, Solid-phase microextraction (SPME) with GC/FID was studied as a possible alternative to liquid-liquid extraction for the analysis of chlorinated solvents (PCE and TCE) and these by-products (cis-DCE, VC, and Ethylene). Experimental parameters affecting the SPME process (such as kind of fibers, adsorption time, desorption time, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. Experimental parameters such as CAR/PDMS, adsorption time of 20 min, desorption time of 5 min at $250^{\circ}C$, headspace volume of 50mL, sodium chloride (NaCl) concentration of 25% combined with magnetic stirring were selected in optimal experimental conditions for analysis of chlorinated solvents and these by-products. The general affinity of analytes to CAR/PDMS fiber was high in the order PCE>TCE>cis-DCE>VC>Ethylene. The linearity of $R^2$ for chlorinated solvents and these by-products was from 0.912 to 0.999 when analyte concentrations range from $10{\mu}g/L$ to $500{\mu}g/L$, respectively. The relative standard deviation (% RSD) were from 2.1% to 3.6% for concentration of $500{\mu}g/L$ (n=5), respectively. Finally, the limited of detection (LOD) observed in our study for chlorinated solvents and these by-products were from $0.5{\mu}g/L$ to $10{\mu}g/L$, respectively.

• Journal of the Korean Society of Food Science and Nutrition
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• v.42 no.9
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• pp.1345-1350
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• 2013

The objective of this study was to evaluate the effect of extraction methods on the antioxidant activity of Citrus unshiu pomace. For this purpose, two kinds of citrus pomace (CP)s, whole fruit CP and pulp CP, were used for preparing the extracts with hot water or 70% ethanol. It is well-known fact that whole fruit CP has more calories and carbohydrates, although moisture content is higher in pulp CP. Further, whole fruit CP extracts have higher levels of total phenolic contents compared to CP extracts. In addition, DPPH and alkyl radical scavenging activities were also higher in whole fruit CP, especially in ethanolic extracts. Our results based on liquid chromatography-mass spectrometer showed that 70% ethanolic extract of whole fruit CP has the maximum levels of nobiletin and tangeretin contents. The levels of naringin, which is known as an antioxidant flavonoid, was determined only in the 70% ethanolic extract of whole fruit CP. This result, however, is consistent with the observed DPPH and alkyl radical scavenging activities. We had also performed a gas chromatography analysis that showed all the four extracts contained the compound hydroxymethyl furfural. Significantly, this compound has been reported to have antioxidant activity. Taken together, findings of this study indicate that ethanolic extraction of whole fruit CP is a good source of antioxidant compounds and hence the same could be utilized as an important method to obtain such beneficial compounds on an industrial scale.

• Korean Journal of Food Science and Technology
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• v.32 no.5
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• pp.1029-1034
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• 2000

A suitable method of sample treatments to minimize the analytical interferences was presented in order to determine bisphenols [bisphenol F (BPF), bisphenol A (BPA), bisphenol F diglycidyl ether (BFDGE), and bisphenol A diglycidyl ether (BADGE)] in various canned beverages coated with epoxy resin by the reversephase high performance liquid chromatography (RP-HPLC) equipped with a fluorescence detector and the gas chromatography with mass selective detection. The recovery test of bisphenols was performed using 1, 5, and 10 ${\mu}g/L$ bisphenols spiked beverages with the combined technique of the solid-phase extraction (SPE) and the liquid-phase extraction (LPE). Both BPA and BADGE showed quite adequate resolutions in HPLC-chromatograms. The recoveries of BPA obtained by LPE with diethyl ether were higher than those obtaind with methylene chloride on coffee, shikhye and fruit juice. For cola and tea, the recoveries of BPA obtaind by SPE were higher than those by LPE with diethyl ether. The recoveries of BADGE were less than those of BPA for all beverage samples treated by either SPE or LPE method. In survey of bisphenols for eighteen commercial canned beverage samples, BPA contents of coffee, cola, tea, shikhye, and fruit juice were in the range of $1.3{\sim}11.6,\;0.5{\sim}0.9,\;1.0{\sim}1.3,\;2.4{\sim}7.9$, and $3.0{\sim}3.4\;{\mu}g/L$, respectively, but there was no detection of BPA in beer sample.

• Analytical Science and Technology
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• v.21 no.5
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• pp.412-423
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• 2008

A procedure based on solid-phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry has been developed for the simultaneous analysis of 55 basic drugs in equine urine. The test scope covers diversified classes of drugs including some ${\beta}$-blockers, ${\beta}$-agonists, antihypotensives, CNS stimulants, sedatives, tranquilizers, antidepressants, antihypertensives and so on. LC-MS/MS separation and quantification was carried out in positive electrospray ionization and multiple reaction monitoring (MRM) mode. Four different brands of mixed mode cation exchange SPE sorbents; UCT XTRACT$^{(R)}$ XRDAH, Supelco DSC-MCAX$^{(R)}$, Varian Bond Elut Certify$^{(R)}$ and Waters Oasis$^{(R)}$ MCX were compared. The UCT XTRACT$^{(R)}$ XRDAH sorbent provided the best results in the preconcentration of samples, yielding relative recoveries higher than 80% except for terbutaline (41.3%), salbutamol (71.5%), heptaminol (70.7%), phenylpropanolamine (66.3%). Detection limits of the target drugs provided by the proposed analytical procedure were between 0.2~8.3 ng/mL.

• Analytical Science and Technology
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• v.21 no.6
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• pp.459-473
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• 2008

Antifouling agents including tributyltin (TBT) compound and its derivatives have been used for many years, but the usage of TBT in Korea was legally restricted in 2003, due to its significant environmental impact. Following this, many new alternative antifouling agents have been used. In this experiment, four major antifouling agents were selectively analyzed to study their release in seawater and tidal flats on the Korean Peninsula. These new antifouling agents were extracted from the seawater and tidal flats using a liquid-liquid extraction method and microwave extraction, respectively. The measured concentrations of Irgarol 1051, Sea-Nine 211, Dichlofluanid and Chlorothalonil ranged from N.D.$-23.80ng/{\ell}$, N.D.$-15.30ng/{\ell}$, N.D.$-61.69ng/{\ell}$ and N.D.$-4.19ng/{\ell}$ in the seawater samples and from N.D.-159.45 ng/g, N.D.-476.57 ng/g, N.D.-59.79 ng/g and N.D.-21.27 ng/g in the tidal flat samples, respectively. Interestingly, these new antifouling agents were not detected in any area in the tidal flats at Pusan, whereas a certain amount of them was found in the seawater.

• Analytical Science and Technology
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• v.33 no.1
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• pp.11-22
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• 2020

When extracting semi-volatile components of herbal medicines using hot water vapor, some substances may react with water vapor or oxygen, and some volatile substances may be lost, when using an organic solvent extraction method has the disadvantage that it may contain a non-volatile material and residual organic solvent. In addition, it is inefficient to separate semi-volatile substances from herbal medicines into each single component and conduct biological activity research for each component to determine the effective ingredient, and some components may be lost in the separation process. In this study, semi-volatile substances evaporated under two pressure-reduced conditions in Chinese herbal medicines such as Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus were separated by cooling with liquid nitrogen. Those were analyzed by gas chromatography-mass spectrometry (GC-MS) to identify the components, and this method may be used to study biological activities at the cellular level. The substances separated under reduced pressure, essential oil obtained by simultaneous distillation extraction (SDE) method and substances by using solid phase micro-extraction (SPME) from Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus were analyzed by GC-MS. In the case of Cnidii Rhizoma and Aucklandiae Radix, there were some differences among the essential oil components obtained by SDE and those identified by low temperature capture (CT) and SPME method, these were believed to be produced by some volatiles reacting with water or oxygen at the boiling point temperature of water.

• Korean Journal of Environmental Agriculture
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• v.39 no.2
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• pp.142-169
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• 2020

BACKGROUND: A new analytical method has been developed to determine 261 pesticide residues in herbal medicines. METHODS AND RESULTS: The extraction of pesticides was carried out by modified method of the Korea Food Standards Codex sample extraction and determination was performed using GC-MS/MS and LC-MS/MS. During the pre-treatment process of the test method, Solid-liquid separation was changed to centrifugation. The method was validated by the precision and accuracy results. 261 pesticides spiked at three level 20, 50, 100 ug/kg in herbal medicines. The limit of quantification of method were 4-40 ug/kg for GC-MS/MS and 2-45 ug/kg for LC-MS/MS, respectively. Among the pesticides analysed by GC-MS/MS and LC-MS/MS, 244 pesticides (94% of total number) in chinese matrimony vine and 224 pesticides (86% of total number) in korean angelica root and 231 pesticides (89% of total number) in jujube and 214 (82% of total number) in cnidium showed recoveries in the range of 70-120% with RSD⪯20%. CONCLUSION: These results indicated that GC-MS/MS and LC-MS/MS analysis with the sample extraction in this study can be applied to multi-residue analysis of pesticides in herbal medicines.

• Food Science and Biotechnology
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• v.18 no.3
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• pp.793-798
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• 2009

The objectives of this present study were to compare the contents and determine optimum extraction conditions for the rosmarinic acid (RA) and caffeic acid (CA) from leaves of Korean Perilla frutescens varieties. RA and CA from leaves of cv. Bora, a breeding line of P. frutescens were isolated and elucidated using various spectroscopic data. On the basis of 2 phenolic acids, optimum extraction conditions were obtained by employing 50% EtOH for 60 min at $25^{\circ}C$. We reported for the first time on the contents of RA and CA from leaves of 32 Korean varieties. Among them, leaves of P. frutescens Brit. var. acuta Kudo I exhibited the highest RA content ($8.53{\pm}0.57$ mg/g) and CA content ($2.33{\pm}0.11$ mg/g) showed the highest in the P. frutescens Brit. var. viridis Makino. Interestingly, average RA content ($2.66{\pm}0.17$ mg/g) showed a markedly higher than that of CA ($1.98{\pm}0.16$ mg/g) in Korean varieties. These results suggest that concentrations of the RA and CA in P. frutescens leaves could be a key factor in the selection process of a high quality species.

• Journal of Korean Society of Environmental Engineers
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• v.35 no.2
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• pp.75-83
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• 2013

We applied a sensitive method based on on-line solid-phase extraction (SPE) and liquid chromatography/mass spectrometry (LC/MSD) using an electrospray interface for the determination of eleven perfluorinated compounds (PFCs) in water. The on-line connection suppressed the target loss by keeping the cartridge from drying, which resulted in improvement of the recovery and saving of the analytical time. For the on-line solid-phase extraction of 10 mL water samples, recoveries were between $80.4{\pm}5.2%{\sim}109.5{\pm}1.4%$ and limit of quantification (LOQ) were 3.6~15.9 ng/L for the PFCs. The total PFCs concentrations of the tributaries and main stream of Nakdong River water samples were in the range of $8.0{\sim}678.6{\mu}g/L$.

• Applied Biological Chemistry
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• v.40 no.5
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• pp.442-446
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• 1997

A new analytical method was developed by HPLC after supercritical fluid extraction and fluorogenic derivatization for the determination of quinclorac (3,7-dichloro-8-quinoline carboxylic acid) in soil. The graminicide quinclorac was extracted from soil by supercritical fluid extraction. Supercritical carbon dioxide at 7000 psi $(80^{\circ}C)$ modified with 30% of methanol extracted quinclorac from soil samples at the level of $0.1ng\;g^{-1}$ with 96% recovery. Extracted quinclorac was determined by HPLC as a fluorescent derivative. Derivatization was made with 4-bromomethyl-7-methoxycoumarin (4-Br-Mmc) using 18-crown-6-ether as a catalyst. The conversion was completed within 30 min and the limit of detection was 0.5 ppb to prove that the procedure could be used in the residue analysis of the pesticides containing carboxylic acid group.