• Korean Journal of Food Science and Technology
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• v.38 no.6
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• pp.730-737
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• 2006

High performance liquid chromatographic methods for the simultaneous determination of 12 biogenic amines were developed and contents of biogenic amines in 23 varieties of Korean commercial fermented food were analyzed. Dansyl derivatives of biogenic amine were very stable and had good peak resolution. Except agmatine, the recovery of biogenic amines from soybean paste with extraction of 0.1 N HC1 added biogenic amines to soybean paste was greater 85%. The calibration curve showed good linearity over a concentration range up to 50 ${\mu}g/mL$. In the determination of biogenic amine level in Korean commercial fermented foods, doenjang and chungkukjang (fermented soybean pastes), soy sauce, anchovy and pacific sand lance liquid jeotkal (fermented fish sauce products), and cabbage kimchi had high level biogenic amines. Especially, traditional doenjang had a histamine (HIS) level of 952.0 mg/kg, a tyramine (TYR) level of 1,430.7 mg/kg. Most cheese had low level of biogenic amines, but one Gouda cheese had a tyramine (TYR) level of 97.5 mg/kg. A low level of biogenic amines was detected in wines, beer, yoghurt, and sausage. Putrescine (PUT), cadaverine (CAD), tryptamine (TRY), histamine (HIS), tyramine (TYR), and 2-phenylethylamine (PHE) were mainly formed in fermented foods by the action of microorganism, so their levels were high with a range. On the other hand, spermidine (SPD), spermine(SPM), serotonin (SER), noradrenaline (NOR), and dopamine (DOP) were formed originally via biosynthesis with consequent low level.

• 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.

• The Korean Journal of Pesticide Science
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• v.16 no.4
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• pp.273-281
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• 2012

This study was conducted for the establishment of the analytical method of pesticide residues in rice straw for 9 pesticides; etofenprox, tricyclazole, diazinon, edifenphos, propiconazole, carbaryl, carbofuran, 3-hydroxy carbofuran and 3-keto carbofuran and for the monitoring of these pesticides in rice straw for livestock feed in Korea. These pesticides were classified into 4 groups according to analytical instrument condition. Group 1 (HPLC-UVD1) included tricyclazole and etofenprox while group 2 (HPLC-UVD2) included propiconazole and edifenphos. Group 3 (HPLC-FLD) included carbaryl, carbofuran, 3-hydroxy carbofuran and 3-keto carbofuran. Group 4 (GC-NPD) included Diazinon. The dried rice straw samples were extracted with acetone and purified by liquid-liquid partition and solid phase extraction (SPE): Combination of Florisil SPE and amino-propyl SPE was used for group 1 and group 2, amino-propyl SPE for group 3, and Florisil SPE was for group 4. Recovery was in the ranged 70~110% and the limits of quantitation (LOQ) were lower than the half of maximum residue limits. Therefore this method was proved to be efficient for monitoring of these pesticides residue in rice straw. A total of 18 rice straw samples from 6 provinces in Korea in 2010 were analyzed using established method and, only 3-keto carbofuran was detected in one sample at concentration of 0.04 mg/kg.

• Korean Journal of Food Science and Technology
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• v.31 no.6
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• pp.1471-1476
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• 1999

A simple and practical method for determination of caffeine in foods was developed. The analysis of caffeine was performed by reverse phase high performance liquid chromatography using a ${\mu}-Bondapak\;C_{18}$ column at isocratic condition with methanol-acetic acid-water(20 : 1 : 79) on UV detector at 280 nm. The clean-up and extraction of caffeine in samples were based on a simple pretreatment using a Sep-Pak $C_{18}$ cartridge. Recovery rates obtained with this method for cider, candy, cookie, milk, ice cream and persimmon leaf tea were 99.23%, 99.50%, 99.17%, 99.37%, 98.93% and 99.10% respectively. And the detection limit of caffeine was $0.1\;{\mu}g/mL$. With this method, the range of caffeine contents extracted from coffee, green tea, black tea, Oolong tea(tea bag), soft drinks, ice cream, milk and commercial confectionery were $3.38{\sim}37.50\;mg/g,\;16.30{\sim}26.10\;mg/g,\;10.80{\sim}16.65\;mg/g,\;11.25\;mg/g,\;0.06{\sim}0.11\;mg/g,\;0.04{\sim}0.44\;mg/g,\;0.04{\sim}0.39\;mg/g\;and\;0.10{\sim}1.80\;mg/g$, respectively. But caffeine was not detected in the other tea such as Acanthopanax sessiliflorum tea, Angelica gigas tea, Angelica tea, Arrow root tea, Duchu'ng tea, Dunggulle tea, Ganoerma lucidum tea, Ginger tea powder, Persimmon leaf tea, Ssanghwa tea and Cocoa mix powder.

• Journal of Food Hygiene and Safety
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• v.19 no.1
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• pp.12-18
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• 2004

Ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin in chicken muscle were seperated by liquid extraction and determined with high performance liquid chromatography (HPLC) with fluorescence detector. Analysis was carried out using following conditions; Cl8 column (250${\times}$4.6 mm i.d. 5 ${\mu}{\textrm}{m}$ particle size), mobile phase composed of D.W. (containing 0.4% triethylamine and phospholic acid): methanol : acetonitrile (800:100:100, v/v/v), isocratic pump at a flow rate of 1.0 $m\ell$/min and 50 ${mu}ell$ of injection volume, fluorescence detector with EX278 nm/EM.456 nm. The calibration curves of four fluoroquinolones showed linearity (${\gamma}$$^2$$\geq$0.999) at concenration range of 0.025-0.6 $\mu\textrm{g}$/ml. The recoveries in fortified chicken muscle represented more than 80% with low coefficient of variation (〈10%) for concentration range of four fluoroquinolones. The detection limits for ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin were 23.5, 3.4, 3.0 and 2.5 ng/g in chicken muscle, respectively. We also monitored fluoroquinolones residue in muscle of chickens (broiler 1:227, Korean native chicken 219, laying chicken 77) using EEC-4-plate screening and HPLC conformation methods. Ten(broiler 5, Korean native chicken 5) out of the fifteen samples which were positively detected by EEC-plate screening method from 1,523 chicken meat were confirmed with ciprofloxacin and enrofloxacin by HPLC. The ranges of residual concentration were 0-0.12 ppm for ciprofloxacin and 0.01-6.79 ppm for enrofloxacin. In conclusion, our method could be applied effectively to determine four fluoroquinolones residues in chicken meat, and further survey for fluoroquinolones residue in chicken meat are needed for more effective control of fluoroquinolones used in livestock.

• Analytical Science and Technology
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• v.31 no.6
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• pp.247-258
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• 2018

The purpose of the present study was to investigate whether the degree of air pollution can be evaluated via examination of local plants. Selected sites included two parks in an industrial area, as well as two parks in an urban area. Selected plant samples comprised one-year-old pine shoot leaves. Leaves growing over 2 m from the ground were collected from over 10 pine trees. Leaf surface was analyzed for deposition of 14 trace elements and 16 polycyclic aromatic hydrocarbons (PAHs), including particle size and mass, surface imaging, precipitation-mediated particle removal rate, and concentration. Particle size ranged from 0.4 to $200{\mu}m$, and the volume percentage of particles ${\leq}10$ was 20 %. Deposited particle mass ranged from 0.450-0.825 mg, and precipitation-mediated removal rate ranged from 10.0-27.6 %. Trace element concentration, as measured by ICP/MS after microwave acid digestion, was 18.8-26.3 mg/kg As, 0.08-0.13 mg/kg Be, 0.06-0.08 mg/kg Cd, 4.91-17.8 mg/kg Cr, 5.26-405 mg/kg Cu, 1,930-2,670 mg/kg Fe, 3.03-28.1 mg/kg Pb, 26.9-42.8 mg/kg Mn, 2.66-10.4 mg/kg Ni, 4,560-8,730 mg/kg Al, 2,500-6,120 mg/kg Ba, 5.27-17.8 mg/kg Rb, 40.9-95.3 mg/kg Sr, and 4,030-8,260 mg/kg Zn. Concentration of PAHs, as analyzed by GC/MS/MS after liquid-liquid extraction and purification of deposited particles, ranged from 1.17 to 12.378 mg/kg for ${\Sigma}PAH_{16}$ and from 1.17 to 12.378 mg/kg for ${\Sigma}PAH_7$.

• Journal of Food Hygiene and Safety
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• v.38 no.5
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• pp.390-401
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• 2023

Major components of lac coloring include laccaic acids A, B, C, and E. The Korean Food Additive Code regulates the use of lac coloring and prohibits its use in ten types of food products including natural food products. Since no commercial standards are available for laccaic acids A, B, C, and E, a standard for lac pigment itself was used to separate laccaic acids from the lac pigment molecule. A standard for each laccaic acid was then obtained by fractionation. To obtain pure lac pigment for use in food by High performance Liquid Chromatography Photo Diode Array (PDA), a C8 column yielded the best resolution among various tested columns and mobile phases. A qualitative analytical method using High Performance Liquid Chromatography (HPLC) Tandem Mass(LC-MS/MS) was developed. The conditions for fast and precise sample preparation begin with extraction using methanol and 0.3% ammonium phosphate, followed by concentration. The degree of precision observed for the analyses of ham, tomato juice and Red pepper paste was 0.3-13.1% (Relative Standard Deviation (RSD%)), degree of accuracy was 90.3-122.2% with r²=0.999 or above, and recovery rate was 91.6-114.9%. The limit of detection was 0.01-0.15 ㎍/mL, and the limits of quantitation ranged from 0.02 to 0.47 ㎍/mL. Lac pigment was not detected in 117 food products in the 10 food categories for which the use of lac pigment is banned. Multiple laccaic acids were detected in 105 food products in 6 food categories that are allowed to use lac color. Lac pigment concentrations range from 0.08 to 16.67 ㎍/mL.

• Journal of Environmental Science International
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• v.4 no.2
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• pp.223-232
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• 1995

New two macrocyclic compounds using as carriers of liquid emulsion menbrame, have been synthesized. These reuslts provide evidance for the usefulness of the theory in designing the systems. The efficiency of selective transport for heavy metal ions have been discussed from the membrane systems that make use of $SCN^-$,<>,$I^-$,CN- and $Cl^-$ ion as co-anions in source phase and make use of $S_2O_3^{2-}$ and $P_2O_7^{4-}$ ion as receiving phase, respectively. The transport rate of M(II) was highest when a maximum amount of the M(II) in the source phase was present as$Cd(SCN)_2$$(P[SCN^-]= 0.40M)$, $Hg(SCN)_2([SCN^-]=0.40M)$ and Pd(CN)$([CN^-]= 0.40M)$. The Cd(II) and Pb(II) over each competitive cations were well transprted with 0.3M-S2032- and 0.3M-P2O74-, respectively in the receiving phase. Results of this study indicate that two criteria must be met in order to have effective macrocycle-mediated transport in these emulsion system. First one must effective extraction of the $M^{n+}$ into the toluene systems. The effectiveness of this extraction is the greatest if locK for $M^{n+}$macrocycle interaction is large and if the macrocycle is very insoluble in the aqueous phase. Second, the ratio of the locK values (or Mn+-receiving phase ($S_2O_3^{2-}$- or $P_2O_7^{4-}$) to $M^{n+}$-macrocycle (($L_1$이나 $L_2$) interaction must be large enough to ensure quantitative stripping of Mn+(($Cd^{2+}$,$Pb^{2+}$)at the toluene receiving Phase interface. $L_1$(3.5-benzo-10,13,18,21-tetraoxa-1,7,diazabicyclo(8,5,5) eicosan) forms a stable ($Cd^{2+}$ and >,$Pb^{2+}$ complexes and $L_1$ is very insoluble in water and its $Cd^{2+}$ and >,$Pb^{2+}$ complex is considerably less stable than $Cd^{2+}$-(S2O3)22- and $Pd^{2+}-P_2O_7^{4-}$ complexes. On the other hand, the stability of the $Hg^{2+}$)+-$L_1$( complex exceed that of the $Hg^{2+}$- (S2O3)22- and Hg2+-P2O74-, and the distribution coefficient of $L_2$(5,8,15,18,23,26-hexaoxa-1,12- diazabicyclo-(10,8,8) octacosane) is much smaller than that of $L_1$. Therefore, the partitioning of Lr is favored by the aqueous receiving Phase, and little heavy metal ions transport is seen despite the large logK for $Hg^{2+}$+-$L_1$ and $Mn^+$($Cd^{2+}$+, $Pb^{2+}$+ and $Hg^{2+}$)-$L_2$ interactions. Key Words : macrocycles, transport, heavy metal, co-anion, source phase, receiveing, complex separation, interaction, destribution coefficient.

• Journal of Food Hygiene and Safety
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• v.25 no.4
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• pp.388-394
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• 2010

Metabolomics aims at the comprehensive, qualitative and quantitative analysis of wide arrays of endogenous metabolites in biological samples. It has shown particular promise in the area of toxicology and drug development, functional genomics, system biology and clinical diagnosis. In this study, analytical technique of MS instrument with high resolution mass measurement, such as time-of-flight (TOF) was validated for the purpose of investigation of amino acids, sugars and fatty acids. Rat urine and serum samples were extracted by selected each solvent (50% acetonitrile, 100% acetonitrile, acetone, methanol, water, ether) extraction method. We determined the optimized liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) system and selected appropriated columns, mobile phases, fragment energy and collision energy, which could search 17 metabolites. The spectral data collected from LC/TOFMS were tested by ANOVA. Obtained with the use of LC/TOFMS technique, our results indicated that (1) MS and MS/MS parameters were optimized and most abundant product ion of each metabolite were selected to be monitorized; (2) with design of experiment analysis, methanol yielded the optimal extraction efficiency. Therefore, the results of this study are expected to be useful in the endogenous metabolite fields according to validated SOP for endogenous amino acids, sugars and fatty acids.

• Asian-Australasian Journal of Animal Sciences
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• v.27 no.7
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• pp.1003-1012
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• 2014

The use of a suitable methodology to quantify the phytate phosphorus ($P_{phy}$) content in both the feed and the excreta from broilers is required to enable accurate calculation of the catalytic efficiency of the phytase supplemented in the feed. This study was conducted to compare 2 analytical methodologies (colorimetry and also high-performance liquid chromatography with a refractive index detector) in order to calculate the phytase efficiency by utilizing the results from the methodology that was shown to be the most appropriate. One hundred and twenty broilers were distributed in a $(4+1){\times}2$ factorial arrangement, corresponding to 4 diets that were equally deficient in P supplemented with increasing levels of phytase (0, 750, 1,500, and 2,250 units of phytase activity - FTU - per kg of feed) plus 1 positive control diet without phytase, supplied to male and female birds. The result indicated that the colorimetric methodology with an extraction ratio of 1:20 (mass of sample in g:volume of the solvent extractor in mL) was shown to be the most adequate. There was no interaction between the phytase level and the sex of the broilers (p>0.05). Males consumed 12% more $P_{phy}$ than did females (p<0.01), but the sex of the broilers did not affect (p>0.05) the excretion and retention coefficient of $P_{phy}$. The increase in the phytase level of the diet reduced (linear, p<0.01) the $P_{phy}$ excretion. The greatest $P_{phy}$ retention was estimated at 87.85% when the diet contained 1,950 FTU/kg (p<0.01), indicating that it is possible to reduce the inorganic P in the formulation at an amount equivalent to 87.85% of the $P_{phy}$ content present in the feed, which, in this research, corresponds to a decrease in 2.86 g of P/kg of the feed.