• 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 Chemical Engineering Research
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• v.49 no.5
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• pp.605-610
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• 2011

Phase holdup characteristics of relatively large and small bubbles were investigated in a three-phase(gasliquid-solid) fluidized bed of which diameter was 0.105 m(ID) and 2.5 m in height, respectively. Effects of gas(0.01~0.07 m/s) and liquid velocities(0.01~0.07 m/s) and particle size($0.5{\sim}3.0{\times}10^{-3}m$) on the holdups of relatively large and small bubbles were determined. The holdups of two kinds of bubbles in three phase fluidized beds were estimated by means of static pressure drop method with the knowledge of pressure drops corresponding to each kind of bubble, respectively, which were obtained by dynamic gas disengagement method. Dried and filtered air which was regulated by gas regulator, tap water and glass bead of which density was $2500kg/m^3$ were served as a gas, a liquid and a fluidized solid phase, respectively. The two kinds of bubbles in three-phase fluidized beds, relatively large and small bubbles, were effectively detected and distinguished by measuring the pressure drop variation after stopping the gas and liquid flow into the column as a step function: The increase slope of pressure drop with a variation of elapsed time was quite different from each other. It was found that the holdup of relatively large bubbles increased with increasing gas velocity but decreased with liquid velocity. However, the holdup showed a local minimum with a variation of size of fluidized solid particles. The holdup of relatively small bubbles increased with an increase in the gas velocity or solid particle size, while it decreased slightly with an increase in the liquid velocity. The holdups of two kinds of bubbles were well correlated in terms of operating variables within this experimental conditions, respectively.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.48 no.6
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• pp.429-433
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• 2003

trans-Resveratrol(3,5,4'-trihydroxystilbene) is phenolic compound present in grapes, wines, and peanuts, has been reported to have health benefits including anticarcinogenic effects, protection against cardiovascular diseases and reduced cancer risk. A simple method for the quantitative extraction of trans-resveratrol from peanut has been developed. Optimal conditions for extraction were investigated. Type of solvent, time, and temperature assayed influenced trans-resveratrol yield. Adequate extraction condition was decided to ethanol/water (80:20v/v) maintained at $25^{\circ}C$ for 45 min. After extraction, the protocol consists of sample preparation using a $\textrm{C}_{18}$ solid-phase extraction (SPE) cartridge after concentrate with rotary evaporator and quantified by reversed phase HPLC using a $\textrm{C}_{18}$ column at 308 nm. Analytical methods for measuring trans-resveratrol in peanut were adapted to isolate, identify, and quantify trans-resveratrol in 11 peanut varieties by HPLC (high-performance liquid chromatography) with UV detector, The 11 peanut varieties content ranged from 0.018 to 1.125 $\mu\textrm{g}/\textrm{g}$ with an average of 0.289 $\mu\textrm{g}/\textrm{g}$. The contents were higher in the seeds with than without testa, regardless of varieties. The trans-resveratrol content was Higher in 110, 130 days after sowing than that of other period.

• Journal of Food Hygiene and Safety
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• v.31 no.5
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• pp.327-334
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• 2016

This study was conducted to establish the standard method for the contents of biotin in milk formulas. To optimize the method, we compared several conditions for liquid extraction, purification and instrumental measurement using spiked samples and certified reference material (NIST SRM 1849a) as test materials. LC-MS/MS method for biotin was established using $C_{18}$ column and binary gradient 0.1% formic acid/acetonitrile, 0.1% formic acid/water mobile phase is applied for biotin. Product-ion traces at m/z 245.1 ${\rightarrow}$ 227.1, 166.1 are used for quantitative analysis of biotin. The linearity was over $R^2=0.999$ in range of $5{\sim}60{\mu}g/L$. For purification, chloroform was used as a solvent for eliminating lipids in milk formula. The linearity was over 0.999 in range of 5~60 ng/mL. The detection limit and quantification limit were 0.10, 0.31 ng/mL. The accuracy and precision of LC-MS/MS method using CRM were 103%, 2.5% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested milk formulas were acceptable contents of biotin compared with component specification and standards for nutrition labeling. The standard operating procedures were prepared for biotin to provide experimental information and to strengthen the management of nutrient in milk formula.

• The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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• v.8 no.3
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• pp.251-261
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• 2003

As a part of an on-going project investigating flux of materials in Gomso Tidal Flat, we have monitored temporal and spatial distribution of nitrogen components(TN, PON, DON, DIN) and have sought the relationships with the freshwater input(tidal range, salinity), the biological activities(chlorophyll-${\alpha}$, TP, DIP, silicate) and the resuspended bottom sediment in seawater(SPM) from 1999 to 2000. TN in seawater was 39.05 $\mu\textrm{m}$ol 1$\^$-1/ (31.03∼42.93 $\mu\textrm{m}$ol 1$\^$-1/) without any statistical difference(p<0.05) between the studied periods. Organic nitrogen (DON and PON) occupied 75％, 95％, 73％, and 75％ in April, August, September and November, respectively. DON and PON have been found within the narrow concentration ranges of 11.30∼16.38 $\mu\textrm{m}$ol 1$\^$-1/ and 13.16∼20.04 $\mu\textrm{m}$ol 1$\^$-1/ in spite of severe environmental differences through the studied periods. Dissolved fractions of nitrogen(DON and DIN) occupied 53∼65％ of TN. Only DIN varied with an evident temporal variability: low concentrations(1.325∼1.616 $\mu\textrm{m}$ol 1$\^$-1/) in August and high enrichment(8.377∼14.65 $\mu\textrm{m}$ol 1$\^$-1/) in September. High consumption rate of DIN by phytoplankton and a long-lasted drought probably induced such low concentration of DIN in August. Eventually heavy precipitation probably introduced plenty of new nitrogen sources into Gomso Bay in September. The portion of PON, DON and DIN in the total nitrogen was 40％, 38％ and 22％, respectively. Their contents were in the order of DON>PON>DIN for the year round except PON>DON>DIN only in September. The highest DON portion in August probably due to the active microbial decomposition of organic material in summer. Only in April, some evident negative correlations have been found between chlorophyll-${\alpha}$ and DIN mostly nitrate(-0.64, p<0.01), phosphate(-0.46, p<0.01) and silicate(-0.55, p<0.01). The Si(OH)$_4$/DIN/DIP ratios in the water column suggests the limitation of DIN for the growth of phytoplankton during the dry summer in Gomso Bay, which was the case of August in this work. Even with some difference between the studied periods, the primary factors on the distribution of nitrogen components in seawater overlying the Gomso Tidal Flat have been the tidal range and the freshwater input, but the additional variations were due to the biological activities.

• The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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• v.16 no.2
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• pp.81-96
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• 2011

Sediment oxygen demand(SOD) and denitrification rates were measured in four major estuaries(Suncheon Bay, Seomjin river estuary, Goseong stream estuary and Masan Bay) in south coast of Korean peninsula from March of 2009 to May 2010 to estimate organic matter cleaning capacity. SOD was estimated from the temporal dissolved oxygen concentration change and isotopic pairing technique was employed to measure denitrification. Sediment oxygen demand(SOD) was ranged from -5.1 to 24.6 mmole $O_2m^{-2}d^{-1}$ and denitrification rate was ranged from 0.0 to 3.9 mmole $N_2m^{-2}d^{-1}$in the study area. SOD was the highest in Masan Bay(-2.2 to 19.2, average = 10.2 mmole $O_2m^{-2}d^{-1}$) and Suncheon, Goseong, Tae-an and Seomjin followed. Denitrification was also the highest in Masn Bay(0.0 to 3.9, average = 1.0 mmole $N_2m^{-2}d^{-1}$) and Goseong, Seomjin, Suncheon and Taean followed. The effect of benthic photosynthesis by microphytobenthos on denitrification was evident in some season of Tae-an, Seomjin, and Masn Bay. The increased oxygen level produced by photosynthesis stimulated nitrification without severe adverse effect on denitrification and, as a result, coupled nitrification and denitrification was enhanced in these areas. A difference of seasonal patterns of denitrification at each site depended on relative importance of denitrification on different nitrate source($D_w$: nitrate from water column and $D_n$: nitrated produced during nitrification). Denitrification was maximum during spring in Goseong, Suncheon and Masan Bay. On the contrary, denitrification was the highest during summer in Tae-an and Seomjin estuary.

• Journal of Food Hygiene and Safety
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• v.26 no.1
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• pp.16-24
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• 2011

A method was established for the simultaneous determination of sugar alcohols, erythritol, xylitol, sorbitol, inositol, mannitol, maltitiol, lactitol and isomalt by High Performance Liquid Chromatography (HPLC). The sugar alcohols were converted into strong ultraviolet (UV)-absorbing derivatives with p-nitrobenzoyl chloride (PNBC). HPLC was performed on Imtakt Unison US-$C_18$ column, using acetonitrile: water (77:23) as a mobile phase and UV detection (260 nm). The calibration curves for all sugar alcohols tested were linear in the 10~200 mg/L range. The average recoveries of the sugar alcohols from three confectioneries spiked at 100 ppm of eight sugar alcohol standards ranged from 81.2 to 123.1% with relative standard deviations ranging fromo 0.2 to 4.9%. The limits of detection (LODs) were $0.5{\sim}8\;{\mu}g/L$ and the limits of quantification (LOQs) were $2{\sim}17\;{\mu}g/L$. Reproducibility of 8 sugar alcohols was 0.28~1.97 %RSD. The results of the analysis of confectioneries showed that 89 samples of 130 were detected and the sugar alcohols content of samples investigated varied between 0.4 and 693.7 g/kg. A method for the simultaneous determination of eight sugar alcohols will be used as basic data for control of sugar alcohols in confectioneries, and quality control in food manufacturing.

• Journal of Korean Society of Environmental Engineers
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• v.32 no.5
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• pp.443-454
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• 2010

Phthalate compounds are widely used as plasticizers in polyvinyl chlororide (PVC) resins and other industrial consumer products, and some of them are known to be endocrine disruptors. In Korea, a number of studies have been carried out for the measurement of phthalates in consumer products and drinking water. However, no data are available for those compounds in the ambient air where the general public are routinely exposed. In this study, we evaluated sampling and analytical methods for the determination of phthalates in the ambient atmosphere. A wide range of phthalates compounds were included in the target analytes, which are dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), butyl benzyl phthalate (BBP), di(2-ethylhexyl) phthalate (DEHP), and di-n-octyl phthalate (DOP). Most of samples were collected using a high volume sampler with a PUF/XAD-2 column/quartz fiber filter and then analyzed by GC/MS. Some of samples were simultaneously collected on XAD-2 using a low-volume sampler, together with high-volume samples. The analytical method applied in this study showed good repeatability and linearity. Quantitative detection limits were estimated from 0.60 to 17.84 ng/$m^3$ in air, depending on individual compounds. The field measurements were carried out at 3 sites located in Sihwa- Banwall industrial areas and a suburban area from January 2007 to November 2007. From the field experiments, DEHP, DMP and DBP appeared to be the most abundant compounds in the ambient air. It was also found that DMP, DEP and DBP were mainly distributed in the vapor phase, while BBP, DEHP and DOP were predominantly associated with the particulate phase. The concentrations of DEHP and DMP in the industrial areas ranged from 45.7 to 1,012.7 ng/$m^3$ and from 7.7 to 375.1 ng/$m^3$, respectively. Overall, the high-volume sampling method was demonstrated to be superior to the low-volume method for the determination of phthalates in the ambient atmosphere.

• Journal of Korean Society of Environmental Engineers
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• v.27 no.4
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• pp.420-430
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• 2005

This study was performed to change the hydrophilic $NH_4Y$-zeolite to the hydrophobic one for removal of VOCs by removing the $Al^{3+}$ in the zeolite-structure to increase the Si/Al ratio, for which the three pelleted $NH_4Y$-zeolite samples were contacted separately with the steam of $400^{\circ}C$, $500^{\circ}C$ and $600^{\circ}C$, respectively, in a stainless steel column for 4 hours. Then extraction of the ex-structure aluminum of the hydrolyzed zeolites with the nitric acids of 0.25, 0.50, 0.75, and 0.10 M at $90^{\circ}C$ in 500 mL-flasks, respectively, according to steam temperature were followed. XRD analysises of the dealuminated zeolites showed that the peaks of the zeolites that had been hydrolyzed with the steams of both $500^{\circ}C$ and $600^{\circ}C$ are distorted more with the increase of the concentration of nitric acid used for extraction of the ex-structure aluminums, however, those hydrolyzed with steam of $400^{\circ}C$ became amorphous phase when treated with the all nitric acids of four concentrations. Also the EDX analysises showed that the BET surface areas and TPVS of the zeolites that had been hydrolyzed with the steam of $600^{\circ}C$ were increased with the concentration of the nitric acid when the nitric acids of 0.25 M and 0.5 M had been used but decreased when the nitric acids of 0.75 M and 1.0 M had been used. These results led to the conclusion that both the $600^{\circ}C$ and $500^{\circ}C$-steam and the 0.5 M-nitric acid are appropriate to change the hydrophilic $NH_4Y$-zeolites to the hydrophobic one, which were proven by the measurement of the benzene and tolune-adsorbing capacities showing the same trend as the BET surface area and TPV The Si/Al ratios and water-adsorbing capacities of the dealuminated zeolites were increased and decreased, respectively, with the concentration of the nitric acids so that it showed that the hydrophobicity is increased.

• Microbiology and Biotechnology Letters
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• v.41 no.2
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• pp.198-206
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• 2013

The five anti-complementary polysaccharides (MFKF-NP, MFKF-AP1${\alpha}$, ${\beta}$, and MFKF-AP2${\alpha}$, ${\beta}$) were separated from hot water extracts of fruiting bodies of Fomes fomentarius by two subsequent column chromatography using DEAE-sepharose FF and Concanavalin A-sepharose 4B. The order of anti-complementary activity was MFKF-AP1${\beta}$ > MFKF-AP1${\alpha}$ > MFKF-AP2${\alpha}$ > MFKF-AP2${\beta}$ > MFKF-NP > Polysaccharide Krestine (PSK). Especially, MFKF-AP1${\beta}$ among those showed the most excellent anti-complementary activity (70% of ITCH50 value at $20{\mu}g/ml$). The monosaccharide composition analysis by gas chromatography indicates that MFKF-AP1${\alpha}$ and ${\beta}$ are a kind of homoxylan consisted mainly of xylose above 97%. Molecular weight of MFKF-AP1${\beta}$, major anti-complementary polysaccharide, was estimated to be about 12,000 by high performance liquid chromatography (HPLC). After the incubation of the serum with MFKF-AP1${\beta}$ in the presence or absence of $Mg^{++}$ and $Ca^{++}$ ions, its anti-complementary activity was investigated. This result indicated that MFKF-AP1${\beta}$ seems to be activator both on the classical and the alternative pathway of complement activation.