• Korean Journal of Environmental Agriculture
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• v.37 no.2
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• pp.104-116
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• 2018

BACKGROUND: This experiment was conducted to establish a simultaneous analysis method for 7 kinds of herbicides in 3 different classes having similar physicochemical property as diphenyl ether(bifenox and oxyfluorfen), dinitroaniline (ethalfluralin and trifluralin), and chloroacetamide (metolachlor, pretilachlor, and thenylchlor) in crops using GC-ECD/MS. METHODS AND RESULTS: All the 7 pesticide residues were extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and directly partitioned into n-hexane/dichloromethane(80/20, v/v) to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. The analytes were separated and quantitated by GLC with ECD using a DB-1 capillary column. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop samples fortified with bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries of the 7 pesticide residues ranged from 75.7 to 114.8% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of the analytes were 0.004 (etahlfluralin and trifluralin), 0.008 (metolachlor and pretilachlor), 0.006 (thenylchlor), 0.002 (oxyfluorfen), and 0.02 (bifenox) mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residues. Therefore, this analytical method was reproducible and sensitive enough to determine the residues of bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin in agricultural commodities.

• Korean Journal of Food Science and Technology
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• v.33 no.3
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• pp.307-312
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• 2001

Flavor compounds in Neungee (sarcodon aspratus) were extracted by simutaneous distillation and extraction (SDE), supercritical fluid extraction (SFE) and headspace method. Flavor compounds obtained by various extraction methods were analyzed with GC and GC-MS. The funtionality of flavor compounds were determined by aroma extract dilution analysis (AEDA) of GC-ofactometry methods. Fifty one flavor compounds were totally identified in Neungee mushroom. However, the numbers of flavor extracted SDE, SFE and headspace were 33, 26 and 17 respectively. The major flavor compounds obtained by SDE, SFE and headspace were 1-octen-3-ol, 1-octen-3-one, 3-octanone, 2-octen-1-ol, 3-octanol, 1-octanol and benzenealdehyde. As the results of sniffing test, the major flavor compounds were found to be fresh mushroom flavor, wood flavor, refreshing sweet flavor, mold flavor, bitter-mushroom and metalic-flavor.

• Korean Journal of Environmental Biology
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• v.36 no.3
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• pp.345-351
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• 2018

An efficient, quick and low-cost extraction and clean up method for the determination of 14 polycyclic aromatic hydrocarbons (PAHs) in the agricultural water samples was optimized using gas chromatography-tandem mass spectrometry (GC-MS/MS). The extraction of the target compounds in water sample was carried out with acetonitrile, followed by partitioning promoted by the addition of salt. As a clean-up procedure, dispersive solid phase extraction was employed to purify the analytes of interest for GC-MS/MS analysis. This method was successfully applied for the quantification of PAHs in real water samples collected for the purpose of monitoring from the waterways located in Chungbuk (15 sites) and Gyeongbuk (6 sites), S. Korea. Phenanthrene (0.54 to $2.53{\mu}gL^{-1}$) was detected in all the water samples collected from both the sites. Fluoranthene was detected in the water samples collected from the two sites in Gyeongbuk province, but other PAHs were not determined in these water sampling sites. Based on these results, the determined PAHs were conducted using an environmental risk assessment. The risk characterization ratios (RCRs) for phenanthrene ranged from 0.37 to 3.21. These RCR values referred to as risk was not controlled because RCR values of some sites were greater than 1. In conclusion, it is proposed that the optimized method in combination with GC-MS/MS could be successfully employed for the determination of PAHs in any environmental samples including water samples.

• Proceedings of the PSK Conference
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• 2003.04a
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• pp.276.3-277
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• 2003

A simple, accurate GC analytical technique for the determination of phthalates. commonly used as plasticizers during the manufacturing process of PVC bags, in blood component preparations was developed and validated. The blood component preparations were extracted with n-hexane. The n-hexane layer was evaporated to dryness and the residue was dissolved in 1 $m\ell$ of n-hexane and analyzed by GC and GC/MS. (omitted)

• Analytical Science and Technology
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• v.17 no.2
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• pp.117-129
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• 2004

Amitrole in environment, difficult to be analyzed by GC or GC/MS due to high polarity and low volatility, was analyzed by LC/ESI/MS in the study. Maximum peak intensity of amitrole in LC/MS/ESI mass spectrum is m/z 85 of protonated molecular ion $(M+H)^+$ with 30V of cone voltage at SIR mode. It was confirmed that ratios between main ion of amitrole, 85 of protonated molecular ion, and m/z 58 fragmented ion of amitrole, had increased corresponding with the increment of cone voltage from 20V to 70V. The isotope molecular weight of amitrole was $86([M+H])^+$ at LC/MS analysis and the mass spectrum ratio between 85 mass and 86 mass was not different by the change of concentration but similar to theoretical ratio(less than 10% standard deviation).The linearity of standard calibration curve under same condition with sample treatment method had $y=1.09354e^6X+26947.2$ and $r^2=0.99$. Recovery rates in water and soil samples were 77.64~83.44% and 71.11~79.44%, respectively. Reliability of the analysis was performed with 5 repeated measurements at each level of standard concentration and the result showed that relative standard deviation was less than 10%; therefore, the extraction and analysis method in the study suggested that it would be reliable to measure amitrole in water and soil media.

• Analytical Science and Technology
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• v.11 no.5
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• pp.321-331
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• 1998

The separation and sample extraction methods of 19 polycyclic aromatic hydrocarbons (PAHs) in water samples were investigated by gas chromatography/mass spectrometry (GC/MS) and some extraction methods involved liquid-liquid extraction, disk extraction and solid-phase extraction methods. The separation of 19 PAHs was possible by partial variation of oven temperature of GC/MS in temperature range $80{\sim}310^{\circ}C$. Extraction procedures of PAHs in water samples were somewhat modified and compared as extraction recoveries and the simplicity of methods. Extraction recoveries of PAHs were 71.3~109.5% by liquid-liquid extraction method. By using disk extraction, good extraction recoveries (80.7~94.9%) were obtained in case of $C_{18}$ disk extraction method by filtration. And extraction recoveries of PAHs by $C_{18}$ solid-phase were in the range of 51.8~77.9%. Method detection limits (S/N=5) of 19 PAHs were in the range of 0.25~6.25 ppb by liquid-liquid extraction and solid-phase extraction and 0.05~1.25 ppb by disk extraction methods.

• Analytical Science and Technology
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• v.26 no.5
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• pp.326-332
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• 2013

Geosmin and 2-methylisoborneol (2-MIB) are volatile organic compounds responsible for the majority of unpleasant taste and odor events in drinking water. Geosmin and 2-MIB are byproducts of blue-green algae (cyanobacteria) with musty and earthy odors. These compounds have odor threshold concentration at ng/L levels. It is needed to develop a sensitive method for determination of geosmin and 2-MIB to control the quality of drinking water. In this study, geosmin and 2-MIB in water samples were determined by gas chromatography-mass spectrometry (GC-MS) with headspace-solid phase microextraction (HS-SMPE). The detection limits of this method were 1.072 ng/L and 1.021 ng/L for geosmin and 2-MIB, respectively. Good accuracy and precision was also obtained by this method. Concentrations of the two compounds were measured in raw waters from Nakdong River in the cyanobacterial blooming season. Water bloom formed by cyanobacteria has been occurred currently in Nakdong River. It is needed to investigate the concentrations of geosmin and 2-MIB to control the quality of drinking water from Nakdong River. Both geosmin and 2-MIB were detected in raw waters from Nakdong River at concentrations ranging from 4 to 24 ng/L and 6 to 16 ng/L, respectively.

• Analytical Science and Technology
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• v.22 no.1
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• pp.44-50
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• 2009

In this study, the use of purge & trap GC-MS technique for determination of methylmercury in sediment samples was described. The method detection limit of the method was determined as 0.06 ng/g and the recovery of the method was $102{\pm}11.4%$, with precisions better than 11.2%. The method was validated by analysis of CRMs such as ERM CC580 (estuarine sediment) and IAEA 405 (sediment). Additionally, the performance of the method was tested on river sediment samples and the analytical results were compared with those of the GC-CVAFS, which has been widely used for methylmercury analysis.

• Analytical Science and Technology
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• v.29 no.1
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• pp.49-55
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• 2016

A ketone body (acetoacetic acid, β-hydroxybutyric acid, and acetone) increases from blood or urine when bio-energy dependence pays more fatty acid than glucose. However, in case oxidation of fat is greater than the capacity of the citric acid cycle the fatty acid oxidation is made from acetoacetyl CoA to acetoacetate then, again form β-hydroxyburytic acid to acetone, the diffusion take place into the blood. Enzymes that oxidize ketone body in the brain and nerve tissue blood ketone dody is increased during prolonged fasting, brain used it as energy. In this study, we developed the rapid two step derivatization method for sensitive detection of the ketone body by GC-MS/SIM. The plasma was deproteinized and then the hydroxy and carboxyl groups of ketone body are subjected to extraction and drying then, keto-group were derivatized with hydoxylamine at 60℃ for 30 min for oximation. Then it was trimetyl-silylated with BSTFA at 80℃ for 30 min and analyzed using a GC-MS. The linear ranges were in between 0.001 μg/mL and 250 μg/mL for β-hydroxy butyrate, and acetoacetate. The method detection limits were below 0.1 pg over each target compound determined. The mean recoveries (%) of target compounds were ranged from 88.2 % to 92.3 % at 1 µg/mL, from 89.5 % to 94.8 % at 10 μg/mL, with RSD of 6.3-9.4 %. This method could be applied to quantification of ketone bodies which are seen in the keto-acidosis in children and adults from a variety of diseases that cause ketones in the blood and urine.

• The Korean Journal of Food And Nutrition
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• v.14 no.1
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• pp.20-27
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• 2001

The consumption of radish ( Rhaphanus sativus L.) sprout, which is Cruciferae family, is increasing because of its pungent flavor and taste. Its volatile components were analyzed by SDE (simultaneous steam distillation & extraction) method and P&T(purge & cryogenic trapping) method. As a solvent, diethyl ether and diethyl ether : pentane mixture(2:1, v/v) were used in SDE method, and diethyl ether in P&T method. Analyzing by GC and GC-MS, the major component was sulfur compounds (19 species, peak area 76.6%) with diethyl ether, sulfur compounds(15. 44.0%) and hydrocarbons(23, 23.8%) with diethyl ether-pentane mixture in SDE method. Also, hydrocarbons(25, 84.1% ) was major component in P& T method. The major volatile component of fresh radish sprout were n-heptane, methyl pentane and that of boiled radish sprout were 4-methylthio-3-butenyl isothiocyanate, methyl mercaptane, 2,3-dimethyl disulfide. Low molecular volatile components were detected more by P& T method, but types and relative quantities of volatile components were measured less comparing to SDE method.