• Bulletin of the Korean Chemical Society
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• v.32 no.8
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• pp.2637-2642
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• 2011

A new ultrasonic-assisted micellar extraction and cloud-point pre-concentration method was developed for the determination of major saikosaponins, namely saikosaponins -A, -C and -D, in Radix Bupleuri by high performance liquid chromatography with evaporative light scattering detection (HPLC-ELSD). The non-ionic surfactant Genapol X-080 (oligoethylene glycol monoalkyl ether) was chosen as the extraction additive and parameters affecting the extraction efficiency were optimized. The highest yield was obtained with 10% (w/v) Genapol X-080, a liquid/solid ratio of 200:1 (mL/g) and ultrasonic-assisted extraction for 40 min. In addition, the optimum cloud-point pre-concentration was reached with 10% sodium sulfate and equilibration at $60^{\circ}C$ for 30 min. Separation was achieved on an Ascentis Express C18 column (100 ${\times}$ 4.6 mm i.d., 2.7 ${\mu}M$) using a binary mobile phase composed of 0.1% acetic acid and acetonitrile. Saikosaponins were detected by ELSD, which was operated at a $50^{\circ}C$ drift tube temperature and 3.0 bar nebulizer gas ($N_2$) pressure. The water-based solvent modified with Genapol X-080 showed better extraction efficiency compared to that of the conventional solvent methanol. Recovery of saikosaponins ranged from 93.1 to 101.9%. An environmentally-friendly extraction method was successfully applied to extract and enrich major saikosaponins in Radix Bupleuri.

• Analytical Science and Technology
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• v.30 no.6
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• pp.319-328
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• 2017

The identification of explosive residues on specimens obtained from an explosion event is a crucial factor for assessing the cause of the explosion. In order to detect the components of explosives, the explosive residues deposited on surfaces are commonly extracted using swabbing materials pre-wetted with an organic solvent. The residues are then analyzed with analytical instruments such as LC/MS and CE/MS. Most conventionally used swabbing media such as cotton swabs or cotton tip swabs seem unsuitable for extracting explosive residues from the surface of a large area of clothes because the swabbing materials tend to be damaged easily, and because only a relatively small amount of explosives is collected. To overcome these problems, we have introduced a novel wiper ($215{\times}210mm$, single layer, Yuhan-Kimberly, Republic of Korea) as a swabbing material to recover representative organic explosives, namely, TNT, RDX, tetryl, HMX, PETN, and NG, from a large area of clothes. Different sides of the wiper, which was folded in half five times, was used to swab the surface of a clothing. We compared this novel wiper with a cotton swab and a cotton tip swab in terms of the recovery efficiency for the aforementioned organic explosives by pre-wetting with methanol, acetone, and acetonitrile, respectively. We identified that this novel wiper collected a significantly higher amount of organic explosive residues than a cotton swab or a cotton tip swab when using methanol as an extracting solvent.

• Tribology and Lubricants
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• v.28 no.6
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• pp.315-320
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• 2012

For proper functioning, general machines usually need lubricant oil as a cooling, cleaning, and sealing agent at points of mechanical contact. The quality of lubricant oil can deteriorate during operation owing to various causes such as high temperature, combustion products and extraneous impurities. In this study, a heavy load stopped during operation, and the oil was analyzed to check whether any impurities were added. Extraction using acetonitrile followed by reaction with BSTFA(bistrimethylsilyl trifluoroacetamide) showed that, trimethylsilylated ethylene glycol was present in the lubricant oil. To quantify the ethylene glycol in the oil, deuterium-substituted ethylene glycol, which acted as an internal standard, was added to the sample and then extracted with the solvent. Next, the extract was reacted with the derivatizing agent(BSTFA) and then analyzed with GC/MS. The detection limit of this method was found to be $0.5{\mu}g/g$ and the recovery of oil containing $20,000{\mu}g/g$ of ethylene glycol was measured to be 94.8%. A damaged O-ring and eroded cylinder liner were found during the overhaul, which implied the leakage of coolant containing ethylene glycol into the lubricating system. The erosion of the cylinder liner was assumed to be due to cavitation of the coolant in the cooling system.

• Journal of the Korean Wood Science and Technology
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• v.16 no.4
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• pp.70-78
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• 1988

To separate and utilize the main components of hardwood (Quercus mongolica) by organosov pulping (ester pulping), chips were cooked at various conditions such as; the solvent ratio (acetic acid: ethylacetate: water, 50:25:25; 33:33:34; 25:50:25), maximum temperature (165, 170, $175^{\circ}C$), and cooking times (2, 2.5, 3 hr). The pulps were bleached by the sequences of CEDED, C/DEDED, PEDED. Lignin, sugars, and acetic acid were separated from black liquor and washing liquors. 1. The selective delignification at optimal pulp yield (43-45%) was obtained by cooking at acetic acid: ethylace tate: water ratio of 33:34:34 for 3 hr at $170^{\circ}C$. But in this case, kappa no. of the pulp was not reduced under 60 points. 2. Kappa no. of the pulp could be dropped by an acetone wash to remove reprecipitated lignin a t cooked pulp. 3. The unbleached pulps had a brightness of 45-50%, whereas the bleached pulps gave at 88-93% brightness. Tensile, burst, and tear strengths of the bleached pulps were lower than those of kraft pulp, especially in tear strength. The pulps which were bleached with CEDED sequence were higher in strengths than another bleaching sequences. 4. Lignin of 90-95%(lignin base on wood)was separated from black liquor and washing liquors, while the purified sugars and recovery of acetic acid were a low. An organic phase composed of acetic acid, ethylacetate, and water was separated to a two-phase system by proper adjustment of the solvent ratios.

• Korean Journal of Environmental Agriculture
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• v.39 no.1
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• pp.44-49
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• 2020

BACKGROUND: Benzo(a)pyrene is a highly toxic substance which has been listed as a Group I carcinogen by the International Agency for Research on Cancer. There have been numerous studies by researchers worldwide on benzo(a)pyrene. Soxhlet, ultrasound-assisted, and liquid-liquid extractions have been widely used for the analysis of benzo(a)pyrene. However these extraction methods have significant drawbacks, such as long extraction time and large amount of solvent usage. To overcome these disadvantages, we aimed to establish a rapid residual analysis of benzo(a)pyrene content in agricultural products and soil samples. METHODS AND RESULTS: A Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method was used as the pretreatment procedure. For rapid residual analysis of benzo(a)pyrene, a modified QuEChERS method were used, and the best codition was demonstrated after various performing instrument analysis. The extraction efficiency of this method was also compared with Soxhlet extraction, the current benzo(a)pyrene extracting method. Although both methods showed high recovery rates, the rapid residual analysis method markedly reduced both the measurement time and solvent usage by approximately 97% and 96%, respectively. CONCLUSION: Based on these results, we suggest the rapid residual analysis method established through this study, faster and more efficient analysis of residual benzo(a)pyrene in major agricultural products such as rice, green and red chili peppers and also soil samples.

• Korean Journal of Environmental Agriculture
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• v.2 no.2
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• pp.73-77
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• 1983

Principle of steam distillation has been successfully applied to the routine extraction of organochlorine pesticide residues from soil samples. Recovery of 8 organochlorine insecticides was found consistent and also comparable to that of conventional solvent extraction method. Recoveries of ${\alpha}-BHC$ and heptachlor was, however, rather poor at 47 and 45% respectively. The steam distillation method offers added advantages such as economy in time and costly solvents.

• Bulletin of the Korean Chemical Society
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• v.34 no.11
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• pp.3444-3450
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• 2013

Three phase hollow fiber-liquid phase microextraction (HF-LPME), which is faster, simpler and uses a more environmentally friendly sample-preparation technique, was developed for the analysis of Non-Steroidal Anti-Inflammatory Drugs (NSAIDs) in human urine. For the effective simultaneous extraction/concentration of NSAIDs by three phase HF-LPME, parameters (such as extraction organic solvent, pH of donor/acceptor phase, stirring speed, salting-out effect, sample temperature, and extraction time) which influence the extraction efficiency were optimized. NSAIDs were extracted and concentrated from 4 mL of aqueous solution at pH 3 (donor phase) into dihexyl ether immobilized in the wall pores of a porous hollow fiber, and then extracted into the acceptor phase at pH 13 located in the lumen of the hollow fiber. After the extraction, 5 ${\mu}L$ of the acceptor phase was directly injected into the HPLC/UV system. Simultaneous chromatographic separation of seven NSAIDs was achieved on an Eclipse XDB-C18 (4.6 mm i.d. ${\times}$ 150 mm length, 5 ${\mu}m$ particle size) column using isocratic elution with 0.1% formic acid and methanol (30:70) at a HPLC-UV/Vis system. Under optimized conditions (extraction solvent, dihexyl ether; $pH_{donor}$, 3; $pH_{acceptor}$, 13; stirring speed, 1500 rpm; NaCl salt, 10%; sample temperature, $60^{\circ}C$; and extraction time, 45 min), enrichment factors (EF) were between 59 and 260. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of 5-15 ng/mL and 15-45 ng/mL, respectively. The relative recovery and precision obtained were between 58 and 136% and below 15.7% RSD, respectively. The calibration curve was linear within the range of 0.015-0.96 ng/mL with the square of the correlation coefficient being more than 0.997. The established method can be used to analyse of NSAIDs of low concentration (ng/mL) in urine.

• Resources Recycling
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• v.24 no.4
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• pp.50-55
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• 2015

In this study, we have investigated solvent extraction of Ga and recovery of high pure Ga solution from MOCVD dust for manufacturing of LED chip. Effect of extractan, concentration of extractant were examined for choosing the more effective extractant and high pure Ga solution was fabricated by multi-stage extraction/stripping process. For extraction/separation of Ga based on the analysis of raw-material in previous study, 3 different extractants PC 99A, DP-8R, Cyanex 272 has been investigated and the extraction efficiency of 1.5 M Cyanex 272 was 43.8%. It was conformed that extraction efficiency of Ga was 83% in multi-stage extraction and 5N high purity Ga stripping solution without impurities also obtained.

• Resources Recycling
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• v.25 no.5
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• pp.50-56
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• 2016

Extraction behaviour of silver from nitric acid solutions by Cyanex 301 as an extractant was examined. Detailed studies have been conducted to evaluate the effect of different variables influencing the extraction such as concentration of nitric acid and extractant, phase ratio(O/A) and synergism of mixed extractant. The extraction behaviour of associated metals namely Ca, Al, Fe, Zn and Sr has been investigated. The extraction results show that Ag can be extracted effectively by Cyanex 301 and selectively extracted from 3.0M $HNO_3$ using 5% Cyanex 301. Impurity metals loaded in organic phase can be effective scrubbed by 4.0M HCl. Finally, pure silver solution can be obtained efficiently by thiourea as a stripping reagent.

• Natural Product Sciences
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• v.13 no.4
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• pp.378-383
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• 2007

Phenathrene derivatives, such as batatasins, are well-known constituents in Dioscorea Rhizoma. Although phenanthrenes have been reported as representative compounds in this plant, standard markers for quality control have been focused on the polar constituents (saponins and purine derivatives). Herein, simple, rapid and reliable HPLC method was developed to determine 3,5-dimethoxyphenanthrene-2,7-diol (DMP) and batatasin-I (BA-I) as non-polar standard maker compounds of Dioscorea Rhizoma. DMP and BA-I were analyzed under optimized HPLC conditions [column: Columbus $5{\mu}$ C18 100A ($30{\times}4.6mm$ i.d., $5{\mu}m$; mobile phase: $H_2O$ with 0.025% $CH_3COOH$ (v/v) for solvent A and $CH_3CN$ with 0.025% $CH_3COOH$ (v/v) for solvent B, gradient elution; flow rate: 2 mL/min; detection: 260 nm), and each experiment was finished within 13 min. Good linearity was achieved in the range from 0.5 to $10.0{\mu}g/mL$ for each compound, and intra- and inter-day precision were in the acceptable levels. The recovery test were performed with three different Dioscorea Rhizoma samples (D. opposita, D. batatas and D. japonica), and showed its accuracy values in the range of 97.2 - 102.8% for three different concentrations of DMP and BA-I. The content levels of DMP and BA-I were ranged under 0.0020%. These results demonstrated that amounts of DMP and BA-I are easily determined with conventional HPLC-UV-DAD method although the content levels were lower than those of saponins and allantoin in Dioscorea Rhizoma. This HPLC method could be used for quality control of various Dioscorea preparations.