• Food Science and Biotechnology
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• v.18 no.6
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• pp.1515-1518
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• 2009

The objective of this study was to compare 3 extraction methods including, solid phase extraction (SPE), acetonitrile extraction, and methanol extraction, for their usefulness as extraction methods to determine capsaicinoids. The determination of capsaicinoids in the extracts was carried out on a reverse-phased high performance liquid chromatography (HPLC) using a fluorescence detector. Three extraction methods, i.e., SPE, acetonitrile extraction, and methanol extraction were compared for the quantification of capsaicinoids using raw peppers and pepper powder. The highest analytical values were observed using methanol extraction and the lowest values using SPE. Also, the analytical method validation parameters such as accuracy, precision, limit of detection, limit of quantitation, and specificity were calculated to ensure the method's validity. This method provides a fast and accurate approach for the determination of capsaicinoids in peppers.

• 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.

• Asian-Australasian Journal of Animal Sciences
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• v.14 no.10
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• pp.1465-1469
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• 2001

A sensitive high-performance liquid chromatographic method was developed to determine the content of cholesterol in milk and dairy products. To optimize separation of cholesterol, mobile phases including acetonitrile:2-propanol (8:1, v/v), acetonitrile:methanol (3:1, v/v), and acetonitrile:methanoI:2-propanol (7:3: I, v/v/v) were compared. Acetonitrile/methanol/2-propanol was superior to the other mobile phase systems for separating cholesterol. Liquid-liquid extraction (LLE) of cholesterol was simplified using a non-polar solvent, hexane, to remove interfering compounds, and had an excellent recovery $(100{\pm}1.0%)$ of cholesterol. A solid phase extraction (SPE) method using Sep-pak $C_{18}$ was developed and compared with LLE. The SPE method was rapid and highly reproducible. Both extraction methods were useful when used in combination with saponification of esterified cholesterol to facilitate total cholesterol determination. The detection limit of cholesterol was $0.01{\mu}g$. The newly developed HPLC method was rapid, simple, and accurate, and has advantages over the many methods commonly used.

• Analytical Science and Technology
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• v.8 no.4
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• pp.511-517
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• 1995

A cationic water soluble porphyrin (5,10,15,20-tetrakis (l-methyl-pyridinium-4-yl)porphyrin, $H_2tmpyp^{4+}$) and its metalloporphyrins (MP) were easily extracted into acetonitrile separated by addition of sodium chloride ($4mol\;dm^{-3}$) in the presence of sodium perchlorate, where M denotes $Zn^{2+}$, $Cu^{2+}$, $Co^{3+}$, $Fe^{3+}$, and $Mn^{3+}$ and $P^{2-}$ is porphyrinate ion. The extracted ion-pair complexes were completely dissociated to $[MP(ClO_4)_3]^+$, and $[MP(ClO_4)_2]^{2+}$. The extraction and the dissociation constants were determined by taking into account of the partition constant of sodium perchlorate ($K_D=1.82{\pm}0.01$). The chemical properties of the separated acetonitrile phase as $E_{T(30)}$ and $D_{II,I}$ were determined and compared with other water miscible solvents (acetone, actonitrile, 1,4-dioxane, tetrahydrofuran, 1-propanol and 2-propanol). Furthermore, a sensitive and selective method was proposed for the determination of a subnanogram amount of copper(II) in natural water samples by using the present salting-out method and the porphyrins.

• Food Science of Animal Resources
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• v.21 no.1
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• pp.64-70
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• 2001

The extraction procedure and HPLC condition were modified to analyze the residues of oxytetracycline, sulfamethoxazole and chloramphenicol in pork, simultaneously. The antibacterial agents in pork were extracted with 0.02M EDTA-Mcilivine buffer:ethanol:acetonitrile (5:3:2). After the removal of fat with n-hexane, the extracts were evaporated and purified with Sep-pak $C_{18}$ cartridge column using 0.01M oxalic acid 0.1% (v/v) triethylamine (TEA) in acetonitrile. The peak of antibacterial agents was detected with $\mu$ Bondapak C18 column, UV detector (280nm) and 0.01M oxalic acid: methanol: acetonitrile (7.5:2.0:0.5). Detection limits for three antibacterial standards were 0.03 ppm. Calibration curves were linear between 0.03 and 2.0 ppm (R$^2$>0.999). When spiked the level of 1.0 ppm of oxytetracycline, sulfamethoxazole and chloramphenicol into meats, the recoveries from meats were 77.3%, 79.7% and 59.3%, respectively. These results showed that the modified extraction method provided good analytical resolution and the recoveries of the above antibacterial agents in meats.

• Applied Chemistry for Engineering
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• v.5 no.6
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• pp.1016-1023
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• 1994

In process of manufacturing acrylonitrile azeotrope of acetonitrile-water was come into being as by-product. For the purpose of recovering acetonitrile through solvent extraction process benzene, toluene, o-xylene, ethylacetate and monochlorobenzene as solvents were selected in order to separate acetonitrile from azeotrope of acetonitrile-water. In this study liquid-liquid equilibrium data were determined and consistency of the experimental data was investigated. The tie line and plait point for solvent(1)-water(2)-acetonitrile(3) system were determined at $25^{\circ}C$. The parameters in the NRTL, UNIQUAC and modified UNIQUAC model were predicted, distribution coefficient and selectivity of each solvent were determined respectively.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.26 no.3
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• pp.307-316
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• 2016

Objectives: In general, NIOSH method 5506 is most widely used for the occupational exposure measurement of PAHs, but 2-4 ring PAHs have poor desorption efficiency, especially for a filter. The purpose of this study was to determine a method to increase the desorption efficiency of 16-PAHs using an ultrasonic extraction procedure. Methods: Test samples prepared spiked XAD-2 tubes and PTFE filters in the range of $0.01-1.0{\mu}g/mL$ for desorption efficiency study. Four different extraction solvents, acetonitrile, acetone, tetrahydrofuran and dichloromethane, were tested in order to select the most suitable solvent for the extraction of the 16 PAHs. The addition of dimethyl sulfoxide and sonication time were considered in order to determine the method with the highest extraction efficiency. All samples were made in three sets and analysis was replicated seven times by HPLC. Results: Acetonitrile and acetone were the optimized as an extraction solvent and desorption efficiency of 2-ring PAHs such as naphthalene, acenaphthylene were increased 3~19% with dimethyl sulfoxide for XAD-2. Acetone was the best extraction solvent for PTFE filter and the desorption efficiency was increased 3~13% for 2- to 4-ring PAHs. The optimum sonication time was 60 minutes and desorption efficiency increased with extraction time. Conclusions: As a result, the best extraction solvent was acetone with dimethyl sulfoxide for ultrasonic extraction procedure and the desorption efficiency of this method was better than NIOSH 5506's. This study could be applied as a method for occupational exposure measurement of PAHs.

• KSBB Journal
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• v.16 no.4
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• pp.327-331
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• 2001

Catechin compounds from the Green tea cultivated in Bosung (Chollanamdo) were extracted using supercritical fluid and various additives, and analyzed by reversed-phase high performance liquid chromatography (RP-HPLC). The chromatographic column was packed with LiChrospher 100RP-18(15 $\mu$m), and water was used as the mobile phase with 0.05% phosphoric acid and acetonitrile. Gradient election was applied to separate EGCG by changing the mobile phase compositions. Comparing the extraction yield of three different types of supercritical fluids, pure CO$_2$, with additives of water and ethanol (5 wt,%), the extraction amount of EGCG was most abundant in the suprcritical CO$_2$with ethanol. However, more was extracted and pure higher purity was achieved by solvent extraction using ethanol.

• Journal of Ginseng Research
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• v.13 no.2
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• pp.198-201
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• 1989

The amounts of panaxynol and panaxydol, which are major polyacetylone compounds In white ginseng were determined by capillary-GC (FID), and the extraction efficiencies when using varictus extraction solvents (petroleum ether, dichloromethane, ether, ethyl acetate, acetone, acetonitrilr and methanol) and various extraction methods (shaking, Soxhlet and reflux) were compared . The GC column was SPB-1 fused silica capillary (0.25 mm id x30 m, Supelco), and the column oven temperature was programmed to rise from $200^{\circ}C$ to $300^{\circ}C$ at the rate of $4^{\circ}C$ per minute. The extraction efficiencies for panaxynol and panaxydol according to extraction souvtints were the highest in methanol and decreased in the order of dichloromethane, acetone, ether, ethyl acetate, acetonitrile and petroleum ether. The extracttion efficiencies for panaxynol and panaxydol according to extraction methods were the highest for reflux and the lowest for shaking, and those with Soxhlet were almost equal to those for reflux. The analytical amounts of panaxynol and panaxydol obtained by reflux with methanol %mere 4.2 and 6.4 mg/g, respectittely in white ginseng.

• Analytical Science and Technology
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• v.17 no.4
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• pp.289-294
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• 2004

A high performance liquid chromatographic method was designed for the quantitative analysis of oxymatrine in Sophora Radix. The separation of oxymatrine was performed by reversed-phase chromatography with a $C_{18}$ column and a buffered aqueous solution containing acetonitrile, and monitored by UV absorption at 215 nm. Extraction of oxymatrine in Sophora Radix was carried out using various solvents and extraction methods. The optimum extraction efficiency for the crushed Sophora Radix was achieved by reflux at $80^{\circ}C$ in 50% ethanol for five hours. Most extraction methods used to complicate pretreatments. In this study, sublimation was employed for a extraction method without going through complicate pretreatments. Sublimation was carried out under high vacuum ($1{\times}10^{-3}$ torr) and at high temperature ($200^{\circ}C$). Extraction efficiency using Sublimation was found to be inferior to other extraction methods.