• Korean Journal of Environmental Agriculture
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• v.42 no.2
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• pp.139-151
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• 2023

Sulfonylurea herbicides are widely used in agriculture because they have a long residual period and high selectivity. An analytical method was developed using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique for simultaneous determination of sulfonylurea herbicide residues in agricultural products by liquid chromatography tandem mass spectrometry and for establishment MRL (Maximum Residue Limit) of those herbicides in Korea. Extraction was performed using acetonitrile containing 0.1% formic acid with MgSO₄ (anhydrous magnesium sulfate) and NaCl (sodium chloride) and the extract was cleaned up using MgSO₄ and C₁₈ (octadecyl). The matrix-matched calibration curves were composed of 7 concentration levels from 0.001 to 0.25 mg/kg and their coefficients of determination (R²) exceeded 0.99. The recoveries of three spiking levels (LOQ, 10LOQ, 50LOQ, n=5) were in the range of 71.7-114.9% with relative standard deviations of less than 20.0% for all the five agriculture products. All validation values met criteria of the European Union SANTE/11312/2021 guidelines and Food and Drug Safety Evaluation guidelines. Therefore, the proposed analytical method was accurate, effective, and sensitive for sulfonylurea herbicide residues determination in agricultural commodities.

• Analytical Science and Technology
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• v.19 no.5
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• pp.415-421
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• 2006

The following concentrations of some PAHs were investigated; [benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene, indeno (1,2,3-c,d)pyrene] in vegetables(n=160) and fruits(n=50). The food samples were purchased at the local markets in Seoul, Chuncheon, Daejeon, Kwangju and Pusan. The samples were radish, onion, bean sprouts, welsh onion, chinese cabbage, spinach, young pumpkin, garlic, cucumber, carrot, lettuce, sesame leaf, tangerine, persimmon, apple, pear and banana. The methodology involved ultrasonic extraction with dichloromethane, clean-up on Sep-Pak florisil cartridges and determination by HPLC/FLD (High Performance Liquid Chromatography/Fluorescence Detector). Overall method recoveries for 8 PAHs spiked into these products ranged from 95 to 102%. The mean level of the following PAHs were determined; benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene and indeno(1,2,3-c,d)pyrene in vegetables and fruits was N.D., 0.014 ng/g, 0.031 ng/g, 0.016 ng/g, 0.019 ng/g, 0.091 ng/g, 0.016 ng/g and N.D., respectively.

• Analytical Science and Technology
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• v.22 no.3
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• pp.210-218
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• 2009

A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was developed and validated for simultaneous determination of amphetamine derivatives and norketamine in human hair. Preparation of hair involves external decontamination, mechanical pulverization, incubation and extraction prior to instrumental analysis. The samples were derivatized using heptafluorobutyric anhydride, and analyzed by GC-MS/MS. The linear ranges were 0.05-20.0 ng/mg for the analytes except for 3,4-methylenedioxyamphetamine, with good coefficients of determination ($r^2$ >0.998). The intra-day and inter-day precisions were within 10.7% and 8.5%, respectively. The intra-day and inter-day accuracies were between -1.6 and 17.0% and -2.6 and 10.5%, respectively. The limits of detections for each analyte were lower than 0.007 ng/mg, while recoveries were 75.9-100.9%. When the method was applied to hair samples obtained from suspected drug abusers, the concentrations in hair samples were 0.97-19.30 ng/mg for methamphetamine and 0.14-2.56 ng/mg for amphetamine.

• Analytical Science and Technology
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• v.21 no.6
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• pp.535-542
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• 2008

A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed for the determination and confirmation of clenbuterol in bovine muscle and milk. Clenbuterol and clenbuterol-D9 using as an internal standard in samples were extracted with ethyl acetate after hydrolysis and evaporated to dryness. The extracts were dissolved in 20% methanol and cleaned using HLB solid-phase extraction cartridge. The analytes were detected by LC-ESI/MS/MS on a $C_{18}$ column. Mass spectral acquisition was done in selected reaction monitoring (SRM) in positive ion mode to provide a high degree of sensitivity. Using MS/MS with SRM mode, the transitions (precursor to product) monitored were m/z 277${\rightarrow}$203 for clenbuterol, and m/z 286${\rightarrow}$204 for internal standard. The limits of quantitation (LOQ) and mean recoveries of clenbuterol in bovine muscle were $0.2{\mu}g/kg$ and 84.3~91.1%, respectively. The LOQ and mean recoveries in milk were $0.05{\mu}g/kg$ and 87.7~98.3%, respectively.

• Journal of the Korean Society of Food Culture
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• v.22 no.2
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• pp.246-253
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• 2007

Mineral and volatile flavor compounds of Pimpinella brochycarpa N., a perennial Korean medicinal plant of the Umbelliferae family, were analyzed by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and simultaneous steam distillation extract (SDE)-gas chromatography mass spectrometry (GC/MS), head space solid phase micro-extraction (HS-SPME)-GC/MS. Mineral contents of the stalks and leaves were compared and the flavor patterns of the fresh and the shady air-dried samples were obtained by the electronic nose (EN) with 6 metal oxide sensors. Principal component analysis (PCA) was carried out using the data obtained from EN. The 1st principal values of the fresh samples have + values and the shady air-dried have - values. The essential oil extracted from the fresh and the shady air-dried by SDE method contain 58 and 31 flavor compounds. When HS-SPME method with CAR/PDMS fiber and PDMS fiber were used, 34 and 21 flavor compounds. The principal volatile components of Pimpinella brachycarpa N. were ${\alpha}$-selinene, germacrene D, and myrcene.

• KSBB Journal
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• v.23 no.4
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• pp.329-334
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• 2008

The antioxidant activity and the qualitative analysis of Acanthopanax sessiliflorum Seeman were studied by partially purified extract using various methods: extraction by using ethanol solutions and temperatures, and absorption to Diaion HP20 column chromatography using 10%, 20%, 40%, 60% ethanol solutions. Major constituents, chlorogenic acid, caffeic acid, eleutheroside E, was determinated by HPLC method in Acanthopanax sessiliflorum S. 10% and 20% ethanol solutions contain chlorogenic acid (3.020$\pm$0.080%, 20.500$\pm$1.150%, respectively). 40% ethanol solution contains caffeic acid and eleutheroside E (12.270$\pm$0.360%, 1.670$\pm$0.140%, respectively). Diaion HP20 fractions (10%, 20%, 40%, 60% ethanol solutions) showed the scavenging activity of radicals and reactive oxygen species with the $IC_{50}$ values of $81.534{\pm}0.992{\mu}g/ml$, $1.748{\pm}0.098{\mu}g/ml$, $11.487{\pm}1.768{\mu}g/ml$, $21.960{\pm}0.547{\mu}g/ml$ against 1,1-diphenyl-2-picrylhydrazly radical and $1713.548{\pm}34.565{\mu}g/ml$, $131.419{\pm}2.235{\mu}g/ml$, $200.681{\pm}2.444{\mu}g/ml$, $757.897{\pm}6.868{\mu}g/ml$ against superoxide radicals in the xanthine/xanthine oxidase system, respectively. Especially, 20% and 40% ethanol fractions showed more antioxidant activity than dl-$\alpha$-tocopherol. These results suggest that Acanthopanax sessiliflorum S. extract and Diaion HP20 fractions may be useful as a potential source of nutraceutical and cosmetic products.

• Korean Journal of Environmental Agriculture
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• v.36 no.3
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• pp.201-210
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• 2017

BACKGROUND: The current study was to monitor of 9 veterinary antibiotics (ceftiofur, clopidol, florfenicol, sulfamethazine, sulfamethoxazole, sulfathiazole, tetracycline, tiamulin, and tylosin) in manure using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive and negative electrospray ionization mode. METHODS AND RESULTS: Sample preparation was carried out using Mcllvaine buffer and citrate salts to adjust the pH of the sample followed by purification with dispersive solid phase extraction (d-SPE). Separation of analytes during LC-MS/MS analysis was conducted using an Eclipse Plus $C_{18}$ column and the mobile phase was in gradient mode with, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations of all tested antibiotics was good, with $R^2$ determination coefficients ${\geq}0.9920$. The limit of detection (LOD) and quantifications (LOQ) were $0.1-67.0{\mu}g/kg$ and $0.4-200.0{\mu}g/kg$, respectively. Analysis of 13 solid and liquid manure samples taken from the Republic of Korea revealed concentrations less than $0.7{\mu}g/kg$ for tiamulin, $1497.6{\mu}g/kg$ for sulfamethazine. CONCLUSION: To monitor 9 veterinary antibiotics from manure samples in 13 provincial areas throughout the Republic of Korea, an analytical method was developed. The developed method was fully validated and successfully applied for monitoring various veterinary antibiotics in manure samples.

• Korean Journal of Agricultural Science
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• v.16 no.2
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• pp.225-238
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• 1989

These studies were conducted to investigate the extraction, purification and characterization of oriental pear (Niitaka. Pyrus pyrifolia Nak.) protease, and the results obtained were as follows: 1. Oriental pear protease was effectively extracted by the method of homogenizing pear pulp with 0.7 volume of 0.1M-sodium phosphate buffer, pH 6.5 containing 5mM-cysteine, 40mM-2-mercaptoethanol and 2mM-EDTA at 10,000 rpm for 5 min. 2. The protease was purified by ammonium sulfate fractionation, Sephadex G-100 filtration and DEAE-Sephadex A-50 column chromatography, and the purified enzyme gave a single protein band on polyacrylamide gel electrophoresis. 3. The specific activity of purified enzyme was 29.65 unit/mg protein and the yield was 7.22%. 4. The moecular weight of the protease was estimated to be about 51,000 by SDS-polyacrylamide gel electrophoresis, and the enzyme had Km value of 54.5 mg/ml for casein. 5. The purified enzyme had a maximum activity at pH 6.0 and $50^{\circ}C$, and was stable from pH 5.5-6.5 and at temperatures below $50^{\circ}C$ 6. Casein was a better substrate for this protease compared to hemoglobin. 7. The enzyme activity was markedly inhibited by p-chloromercuribenzoic acid and heavy metal salts such as $HgCl_2$ and $MnSO_4$ also considerably inhibited the enzyme activity.

• Food Science of Animal Resources
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• v.31 no.6
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• pp.944-951
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• 2011

An improved cholesterol analysis method was developed for powdered infant formula by gas chromatographic separation after liquid-liquid extraction and partition. In the official Korea Food Standard method for cholesterol analysis, the water phase and solvent phase were not well separated in the case of emulsified foods such as powdered infant formulas and baby foods. For the rapid and simple sample preparation method, an optimized direct saponification condition was established for heating temperature, heating time, and KOH concentration. From the results, the optimum conditions were as follows: heating temperature $90^{\circ}C$, heating time 60 min, and 16 M KOH 10 mL for a 2 g infant formula sample; improved separation condition for gas chromatography was as follows: the initial oven condition was $250^{\circ}C$ for 25 min, the oven temperature was increased to $290^{\circ}C$ by $10^{\circ}C$/min ratio, and finally the oven temperature remained at $290^{\circ}C$for 9 min. The developed method could be implemented for the study of cholesterol, providing the advantages of reduced inspection time and cost in emulsified foods such as infant formula.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.37 no.2
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• pp.185-197
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• 1992

Differences in the amount and chemical characteristics of the epicuticular waxes on rice leaves were studied for the active tillering and heading stages of rice varieties differing widely in gross leaf-surface property and genetics. The amount of waxes on surfaces of rice leaf-blades was determined by extraction with chloroform and chemical composition of the waxes was characterized by thin layer chromatography, gas liquid chromatography and infrared spectrophotometry. The amount of waxes varied by variety and significantly with growth stage. The amount at the heading stage was 1.7 to 3.6 mg/g fresh weight of leaves, which was two to three times as much as that at the tillering stage of 0.8 to 1.8 mg/g fresh weight. The waxes consisted of seven chemical classes, namely diols, fatty acids, fatty alcohols, fatty aldehydes, fatty esters, saturated and unsaturated hydrocarbons. Diols and unsaturated hydrocarbons were identified as new chemical classes of the rice epicuticular waxes. The polar constituents such as dials, fatty acids and fatty alcohols and the non-polars such as fatty aldehydes, fatty esters, and saturated and unsaturated hydrocarbons were identified at the heading stage, but at the tillering stage only the non-polar compounds were identified. In the carbon numbers (C) of the chemical classes, diols were composed entirely of C30 and acids were mainly of C30 and C31. In alcohols, primary alcohols were composed of C13 and C32, and the secondary alcohols were of C14, C16 and / or C30 regardless of the rice varieties. The acid portion of fatty esters, mainly composed of C22 and C23, showed low cabon numbers compared with the aldehydes. The alcohol portion of them showed a wide distribution in carbon numbers from C13 to C26 depending on the rice varieties. Hydrocarbons had odd carbon numbers, consisting mainly of C29 and C31.