• Proceedings of the Korean Society of Toxicology Conference
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• 2006.11a
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• pp.65-74
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• 2006

Modem drug discovery requires rapid pharmacokinetic evaluation of chemically diverse compounds for early candidate selection. This demands the development of analytical methods that offer high-throughput of samples. Naturally, liquid chromatography / tandem mass spectrometry (LC-MS/MS) is choice of the analytical method because of its superior sensitivity and selectivity. As a result of the short analysis time(typically 3-5min) by LC-MS/MS, sample preparation has become the rate- determining step in the whole analytical cycle. Consequently tremendous efforts are being made to speed up and automate this step. In a typical automated 96-well SPE(solid-phase extraction) procedure, plasma samples are transferred to the 96-well SPE plate, internal standard and aqueous buffer solutions are added and then vacuum is applied using the robotic liquid handling system. It takes only 20-90 min to process 96 samples by automated SPE and the analyst is physically occupied for only approximately 10 min. Recently, the ultra-high flow rate liquid chromatography (turbulent-flow chromatography)has sparked a huge interest for rapid and direct quantitation of drugs in plasma. There is no sample preparation except for sample aliquotting, internal standard addition and centrifugation. This type of analysis is achieved by using a small diameter column with a large particle size(30-5O ${\mu}$m) and a high flow rate, typically between 3-5 ml/min. Silica-based monolithic HPLC columns contain a novel chromatographic support in which the traditional particulate packing has been replaced with a single, continuous network (monolith) of pcrous silica. The main advantage of such a network is decreased backpressure due to macropores (2 ${\mu}$m) throughout the network. This allows high flow rates, and hence fast analyses that are unattainable with traditional particulate columns. The reduction of particle diameter in HPLC results in increased column efficiency. use of small particles (<2 urn), however, requires p.essu.es beyond the traditional 6,000 psi of conventional pumping devices. Instrumental development in recent years has resulted in pumping devices capable of handling the requirements of columns packed with small particles. The staggered parallel HPLC system consists of four fully independent binary HPLC pumps, a modified auto sampler, and a series of switching and selector valves all controlled by a single computer program. The system improves sample throughput without sacrificing chromatographic separation or data quality. Sample throughput can be increased nearly four-fold without requiring significant changes in current analytical procedures. The process of Bioanalytical Method Validation is required by the FDA to assess and verify the performance of a chronlatographic method prior to its application in sample analysis. The validation should address the selectivity, linearity, accuracy, precision and stability of the method. This presentation will provide all overview of the work required to accomplish a full validation and show how a chromatographic method is suitable for toxirokinetic sample analysis. A liquid chromatography/tandem mass spectrometry (LC-MS/MS) method developed to quantitate drug levels in dog plasma will be used as an example of tile process.

• Korean Chemical Engineering Research
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• v.55 no.2
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• pp.141-155
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• 2017

In the present paper, we investigated the development status of precipitated calcium carbonate (PCC) production using steel slag, which is one of mineral carbonation (MC) technologies, from the standpoint of $CO_2$ utilization. Principle, feature, and global and domestic development status of the mineral carbonation technology were discussed together with the overview of the production method and market of PCC. Mineral carbonation is known as stable and environmentally-friendly technology enabling economical treatment of industrials wastes. Typically, PCC is produced by the reaction of $CO_2$ with supernatant solution after Ca extraction from steel slag followed by the separation of solid and liquid. The development status of MC using steel slag is at the pilot stage (Slag2PCC at Aalto University), and there remains the process economics improvement for commercialization. Key technologies for the further development are efficient extraction of Ca ions from steel slag including impurities removal, valorization of PCC via shape and size control, usage development and value-addition of residual slag, and optimization of reaction conditions for continuous process setup, etc.

• Bulletin of the Korean Chemical Society
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• v.25 no.10
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• pp.1508-1512
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• 2004

A gas chromatography/mass spectrometric (GC/MS) method has been developed for the determination of trace mono-n-butyltin (MBT), di-n-butyltin (DBT), and tri-n-butyltin (TBT) compounds in sediments. Samples were extracted by 10% acetic acid in methanol containing 0.03% tropolone and were then derivatized for GC/MS analysis. Ethylation by sodium tetraethylborate and phenylation by sodium tetraphenylborate were evaluated as a derivatization reaction of the organotins in sample extract. n-Hexane was added into reaction media in the beginning of the reaction for the continuous extraction of derivatized organotins. Ethylation requires less than 2 hours to get proper derivatization yields for MBT, DBT, and TBT altogether and produces relatively low amounts of side reaction products. Compared to ethylation, phenylation requires much longer time but provides relatively lower yield and produces considerable amounts of side reaction products. Therefore, the ethylation reaction was applied for the analysis of organotin compounds in sediment. An isotope dilution mass spectrometric (IDMS) method based on GC/MS has been applied to the accurate determination of DBT compounds in the sediments. The IDMS results from the analyses of sediment samples showed a reasonable repeatability and a good agreement with the values obtained by IDMS based on liquid chromatography/induced coupled plasma/mass spectrometry.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.57 no.4
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• pp.327-335
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• 2024

A simultaneous analytical method was developed to quantify antifouling agents and triazine herbicides in seawater using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The target compounds included diuron, irgarol 1051, and prometryn, which are prevalent in marine environments owing to their extensive use in antifouling coatings and agriculture. The analytical procedure involves solid-phase extraction (SPE) using HLB cartridges followed by LC-MS/MS analysis for precise quantification. The method exhibits high recovery rates for diuron (101% ± 1.25), irgarol 1051 (94.7% ± 2.08), and prometryn (93.7% ± 3.06). Seawater samples from 30 coastal sites in Korea were analyzed. Irgarol 1051 was not detected, whereas diuron was consistently detected across all sites, with concentrations from 0.68 to 11.3 ng/L, and prometryn was present at levels between 0.12 and 7.06 ng/L. The highest diuron and prometryn concentrations were recorded along the southeastern and western coasts, respectively. These findings underscore the critical need for continuous monitoring and regulations to manage these contaminants in marine ecosystems, thereby safeguarding ecological integrity and public health. This study establishes a robust analytical framework for the comprehensive assessment of multiple marine contaminants.

• Journal of the Korean Society of Food Science and Nutrition
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• v.31 no.6
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• pp.958-964
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• 2002

To select the irradiation-induced marker components from volatile flavor compounds in irradiated chicken, and complement the extraction problems of liquid continuous extraction (LLCE) method, the volatile compounds of irradiated (0,1,3,5 and 10 kGy) chicken were analyzed by Purge and Trap (P&T) and gas chromatography/mass spectrometry (GC/MS) methods. A total of 119 compounds were detected in irradiated chicken, and these compounds were composed mainly of 7 aldehydes,22 ketones,8 alcohols,30 esters,36 hydrocarbons,8 aromatic compounds and 8 miscellaneous compounds. Among these, only 21 compounds were detected in both LLCE and P&T methods, and the 98 other were detected in omly P&T method. Among volatile compounds detected in irradiated chicken, only 3 compounds such as hexene (r=0.96, p<0.01), propanol (r=0.93, p<0.05) and 1,3-bis(1,1-dimethylethyl) benzene (r=0.96, p<0.05) were newly selected as marker compounds in irradiated chicken by P&T method, which showed significant and high positive correlation coefficient in the change of relative concentration according to the increment of irradiation dosage.

• Journal of the Korean Society of Food Science and Nutrition
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• v.31 no.4
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• pp.566-571
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• 2002

Volatile flavor compounds in Alaska pollack sik-hae during fermentation at 5$^{\circ}C$ were analyzed by liquid-liquid continuous extraction (LLCE) and gas chromatography/mass spectrometry (GC/MS) methods. Sixty five volatile compounds were detected in Alaska pollack sik-hae during fermentation. These compounds were composed mainly of 11 S-containing compounds, 13 alcohols, 13 acids, 4 aldehydes, 4 ketones, 6 terpenes,4 aromatic compounds and 10 miscellaneous compounds. Among these, 9 S-containing compounds (3-(methylthio)-1-propene, dimethyl disulfide, diallyl sulfide, methylallyl disulfide, methyl-(E) -propenyl disulfide, dimethyl trisulfide, 2 diallyl disulfide isomers and diallyl trisulfide), 2 acids (acetic acid and butanoic acid), 2 ketones (2, 3-butanedione and 6-methyl-5-hepten-2-one) and 2 esters (ethyl formate and ethyl acetate) were significantly increased during fermentation (p<0.05), and these compounds were suspected to affect on the odor of Alaska pollack sik-hae.

• Journal of the Korean Society of Food Science and Nutrition
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• v.29 no.6
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• pp.1050-1056
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• 2000

To identify the irradiation-induced volatile flavor compounds, which were not detected in unirradiated sample and had positive correlation with the increment of irradiation dose, the volatile flavor compounds of irradiated (0, 1, 3, 5, 10 kGy) chicken were analyzed by liquid liquid continuous extraction (LLCE) and gas ehromatographyimass spectrometry (GC/MS) methods. One hundred twenty nine compounds were detected in irradiated chicken, and these compounds were composed mainly of hydrocarbons (62 compounds), aromatic compounds (44), aldehydes (9), ketones (5) and miscellaneous compounds (10). Among these, only 3 volatile compounds including 2-methylpentanal (r=0.24), 4-methylcyclohexene (r=0.08) and cyclotetradecene (r=0.92), were detected as irradiation-induced volatile flavor compounds in irradiated chicken. However, only cyclotetradecene was selected as a marker compound for detecting irradiation dosages with high correlation coefficient in irradiated chicken.

• Journal of the Korean Society of Food Science and Nutrition
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• v.29 no.6
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• pp.1042-1049
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• 2000

Irradiation-induced volatile flavor compounds in irradiated (1, 3, 5, 10 kGy) beef were analyzed by liquid liquid continuous extraction (LLCE) and gas chromatography/mass spectrometry (GC/MS) methods. One hundred fifty volatile compounds were detected in irradiated beef. These compounds were composed mainly of 71 hydrocarbons, 35 aromatic compounds, 15 aldehydes, 7 ketones, 4 acids, 6 esters and 12 miscellaneous compounds. Among these, only 6 volatile compounds including (E) -2-hexenal, nonene, 2-nonenal, cyclodecene, dodecene and cyclododecene were detected as irradiation-induced volatile flavor compounds, comparing with unirradiated beef meat. However, 4 volatile compounds, such as cyclodecene (r=0.88), (E)-2-hexenal (r=0.85), nonene (r=0.74) and 2-nonenal (r=0.70), having a positive correlation coefficient with the increment of irradiation dose, were considered as marker compounds for detecting irradiation dosages in irradiated beef.

• Korean Journal of Food Science and Technology
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• v.37 no.5
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• pp.723-729
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• 2005

Volatile compounds of dropwort (Oenanthe javanica DC), crown daisy (Chrysanthemum coronarium L. var. spatiosum), and sesame (Sesamum indicum L.) were isolated by steam distillation under reduced pressure (DRP) and liquid-liquid continuous extraction (LLE). Aroma extracts of the plants were identified by gas chromatography (GC) and gas chromatography/mass spectrometry (GC/MS) and their antioxidant activities were evaluated in two different assays. The aroma extracts isolated from dropwort, crown daisy, and sesame inhibited the oxidation of hexanal by 25%, 95%, and 99%, respectively, for one month at the $500{\mu}g/mL$ level. They inhibited malonaldehyde formation from cod liver oil by 48%, 54%, and 29%, respectively, at the $500{\mu}g/mL$ level. Their antioxidant activities were comparable to those of the natural antioxidant, ${\alpha}-tocopherol$.

• Journal of Food Hygiene and Safety
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• v.32 no.3
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• pp.187-192
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• 2017

The consumption of herbal medicines has been increasing with growing interest in health. However, due to recent climate change and the complex distribution process of herbal medicines with high import dependence the likelihood of contamination with mycotoxin has been increased. Mycotoxins are emerging as key indicators for ensuring safety of herbal medicines. A total of 498 herbal medicine samples were screened for mycotoxin contamination in this study. Aflatoxin in the herbal medicine samples was extracted by using immunoaffinity column, then the extracted aflatoxin was quantified via high performance liquid chromatography coupled with fluorescence detection (HPLC-FLD) method. The extraction method was verified by linearity, recovery, LOD and LOQ. Aflatoxins were detected in 39/498 samples in an average of $7.670{\mu}g/kg$ ($0.610-77.452{\mu}g/kg$ range). Although safety standards for Corydalis Tuber is not currently available in korea, five of the 39 samples had high concentration of aflatoxins (average of $14.9{\pm}4.1{\mu}g/kg$). In conclusion, it is urgent to establish safety criteria of aflatoxin in Corydalis Tuber. The results of the current study suggest that continuous monitoring is necessary for proactive management of herbal medicine safety.