• Analytical Science and Technology
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• v.13 no.5
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• pp.608-615
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• 2000

A determination method of trace nickel and cobalt in water samples was studied and developed by adsorbing their complexes on ion exchange resin suspension. The analytical ions were formed as complexes with a ligand of APDC (ammonium pyrrolidinedithiocarbamate) and adsorbed on anion exchange resin of Dowex 2-X8. After the suspension was filtered out with membrane filter, the complexes were dissolved in HCl solution by an ultrasonic vibrator for ET-AAS determination. Several conditions were optimized as followings. pH of sample solution: 5.0, amount of ligand APDC: more than 430 times in mole ratio, the type and concentration of acid: 0.1 M HCl, and vibration time: 7 minutes. The addition of palladium in the HCl solution could improve the reproducibility and sensitivity by a matrix modification in the absorbance measurement. This procedure was applied for the analysis of three kinds of real water samples. The detection limits equivalent to 3 times standard deviation of blank were Co 0.36 ng/mL and Ni 0.27 ng/mL and recoveries in spiked samples were 99-102% for cobalt and 100-105% for nickel.

• Korean Journal of Food Science and Technology
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• v.42 no.5
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• pp.541-548
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• 2010

In this study, contamination levels of 7 N-nitrosamine were investigated in processed meat products (n=51), processed fish products (n=62), salted fish pickles (n=20), and beer and malt beverages (n=21) using a GC/PCI-MS/MS method. The limits of detection (LOD) of the N-nitrosamines ranged from 0.2 to 0.5 ${\mu}g$/kg. In addition, methods were used to estimate the recovery of 7 N-nitrosamines, which ranged from 84 to 112%. N-nitrosamines were detected in 89 (58%) out of 154 samples. The exposure of an entire population group to N-nitrosamines through food intake was estimated using the average body weight of the total population and average daily food consumption, to perform risk assessment based on reports of a national health and nutrition survey. The results indicated that the daily intake of N-nitrosamines over a life time was $4.92{\times}10^{-7}$ mg/kg b.w./day. The margin of exposure (MOE) for the general population, estimated using the benchmark dose lower confidence limit 10 ($BMDL_{10}$) of N-nitrosodimethylamine, was 208,939, which was found to be safe.

• Korean Journal of Environmental Agriculture
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• v.12 no.3
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• pp.239-246
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• 1993

In order to clarify the possible contamination of rice straw used as a crude feed for livestock, Korean native cattle and cow, by pesticides, the samples collected from 21 sites in Korea were analyzed by a multiresidue method for 10 pesticides with GLC to obtain the following results. 1. Detection limits were 0.001ppm in butachlor, 0.002ppm in chlorpyrifos, 0.003ppm in BPMC, pirimiphos-methyl and diazinon, 0.004ppm in fenitrothion, 0.005ppm in phenthoate, 0.009ppm in IBP, 0.015ppm in carbofuran, and 0.03ppm in carbaryl. 2. In recovery tests, 73-101% of the pesticides applied were recovered, the recovery being low in carbofuran and chlorpyrifos. 3. Butachlor, 2-chloroacetanilide herbicide, and BPMC, carbaryl, and carbofuran, carbamate insecticides, were not detected in any sample. 4. In organophosphorus insecticides, the amounts of fenitrothion in sample No. 1, 2, 4, 5, 7, 12, 20 and 21 were in the range of 0.01-0.05ppm, those of phenthoate detected in sample No. 10 and 12 were 0.4 and 0.17ppm, respectively, and those of IBP in all samples, with the exception of sample No. 7, 12, 16, 17, 20, and 21, were in the range of 0.01-0.20ppm. The residues of chlorpyrifos, diazinon, and pirimiphos-methyl were not detected.

• Food Science of Animal Resources
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• v.22 no.1
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• pp.50-54
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• 2002

The aim of this work to determine the formation of lactulose during heat treatment process as a contribution to the estabilishment of limits of chemical indicators for different types of heat processed milk and analyze of lactulose for the reconstituted milk added samples. The HTST(75$\^{C}$/15s) and UHT(130$\^{C}$/2∼3s) treatment realized with a pilot plant and heat-treated samples were stroed at 4, 10, 30$\^{C}$ for 4 weeks. Changes in lactulose was evaluated at 7 days intervals. The other heat treatment was sealed in glass tube and heated at 75$\^{C}$ for 10 to 120s and heated at 130$\^{C}$ for 2 to 60s in a thermostatically controlled constant temperature bath of glycerol. The reconstituted milk was made with full fat dry milk that reconstituted with deionized water to 10% total solid, and was added to milk at 10, 20, 30% respectively. The samples processed with a HTST pilot plant showed that lactulose was contained at 1.47∼1.52mg/10()ml and 8.19 ∼8.32mg/100ml for UHT-treated samples. Changes in the lactulose content of heat-treated samples during storage at 4 and 10$\^{C}$ for 4 weeks caused a slight increase, however a noticeable increase was observed at 30$\^{C}$ for 4 week. The glass tube samples showed that high correlations between relative increase in content of lactulose and increasing processing times(75$\^{C}$ : r = 0.986, 130$\^{C}$ : r = 0.987, respectively). Added with reconstituted milk would cause a increase of the lactulose content linear with increasing addition amount(r = 0.982). This results observed for lactulose in commercial milk samples would applied to the detection of chemical changes during heat treatment and illegal use of reconstituted milk.

• Korean Journal of Environmental Agriculture
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• v.1 no.1
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• pp.14-21
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• 1982

Analytical methods for residues of six N-methylcarbamate insecticides were investigated to compare the minimum detectability, recovery from several crops and feasibility of multiple residue analysis. Those methods studied in this work included spectrophotometry by diazotization and gas chromatography by N-trifluoroacetylation(TFA), pentafluorobenzylether(PFB) and dinitrophenylether (DNP) derivatization. Maximum absorbed wavelength of the diazotized MIPC, XMC, BPMC, propoxur and carbofu ran was around 460 ㎚, while that of carbaryl recorded 510 ㎚. Recovery from brown rice and apple by diazotization method ranged from 80 to 120% and minimum detectable limits were 0.03 to 0.05 ppm in 50 g of the sample. Minimum detectability of PFB derivatives by gas chromatography was superior to TFA and DNP derivatives. DNP derivatives showed the longest retention time among the given derivatives. Recovery from crops by gas chromatographic met hod ranged 74 to 94%, 78 to 93%, and 85 to 99% in brown rice, rice straw and apple, respectively. Limit of detection was 0.01 ppm for TFA, 0.005 ppm for PFB and 0.02 ppm for DNP derivatives in 50 g of the crop samples.

• Food Science of Animal Resources
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• v.34 no.6
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• pp.799-807
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• 2014

Meat source fraud and adulteration scandals have led to consumer demands for accurate meat identification methods. Nucleotide amplification assays have been proposed as an alternative method to protein-based assays for meat identification. In this study, we designed Loop-mediated isothermal amplification (LAMP) assays targeting species-specific mitochondrial DNA to identify and discriminate eight meat species; cattle, pig, horse, goat, sheep, chicken, duck, and turkey. The LAMP primer sets were designed and the target genes were discriminated according to their unique annealing temperature generated by annealing curve analysis. Their unique annealing temperatures were found to be $85.56{\pm}0.07^{\circ}C$ for cattle, $84.96{\pm}0.08^{\circ}C$ for pig, and $85.99{\pm}0.05^{\circ}C$ for horse in the BSE-LAMP set (Bos taurus, Sus scrofa domesticus and Equus caballus); $84.91{\pm}0.11^{\circ}C$ for goat and $83.90{\pm}0.11^{\circ}C$ for sheep in the CO-LAMP set (Capra hircus and Ovis aries); and $86.31{\pm}0.23^{\circ}C$ for chicken, $88.66{\pm}0.12^{\circ}C$ for duck, and $84.49{\pm}0.08^{\circ}C$ for turkey in the GAM-LAMP set (Gallus gallus, Anas platyrhynchos and Meleagris gallopavo). No cross-reactivity was observed in each set. The limits of detection (LODs) of the LAMP assays in raw and cooked meat were determined from $10pg/{\mu}L$ to $100fg/{\mu}L$ levels, and LODs in raw and cooked meat admixtures were determined from 0.01% to 0.0001% levels. The assays were performed within 30 min and showed greater sensitivity than that of the PCR assays. These novel LAMP assays provide a simple, rapid, accurate, and sensitive technology for discrimination of eight meat species.

• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.453-462
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• 2011

This study was carried out to survey the residual characteristics of pesticides and assess their safety. Nineteen agricultural commodities, collected from wholesale and traditional markets in Cheongju. Nineteen agricultural commodities including perilla leaves were collected from the markets on October 29th, 2010. Total 240 pesticides which can be analyzed by multiresidue analysis method by GLC and HPLC were monitored and the pesticides detected were confirmed by GC-MSD and LC-MS. Five pesticides, alachlor, bifenthrin, endosulfan, procymidone and triflumizole, were detected from five samples, such as welsh onion, leek and celery in case of wholesale market and perilla leaves and welsh onion in case of traditional market. Detection rate of 13.2% was obtained as a result of pesticide analysis but 2.6% of the pesticides detected exceeded their maximum residue limits. The estimated daily intakes (EDIs) and maximum permissible intakes (MPIs) of the pesticides detected were less than 26% and 0.05% of their acceptable daily intakes (ADIs) respectively, representing that residue levels of the pesticides detected would be safe.

• Journal of the Korean Chemical Society
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• v.39 no.12
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• pp.918-924
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• 1995

THMs and PCBs were separated and analysed with elution on Novapak ODS or $\mu-Bondapak$ phenyl column by an eluent containing p-nitrophenol (p-NP). THMs studied were CHCl3, CHBrCl2, CHBr2Cl, and CHBr3, and PCBs used were Aroclor 1221, 1242, 1248, $\alpha-$ and $\beta-BHC.$ It was thought that the retention on the stationary phase and sensitivities of the samples are related to the interaction between the sample and stationary phase or p-NP. THMs were separated completely on the ODS column by elution with MeOH-water (30 : 70) containing $1.0{\times}10^{-4}$ M p-NP and some of PCBs were separated on the phenyl column by elution with $CH_3CN$-water(50 : 50) containing $1.0{\times}10^{-4}$ M p-NP. Detection limits of THMs were from $1.0{\times}10^{-4}$ g to $1.0{\times}10^{-6}$ g. Aroclors were $2{\times}10^{-6}$ g, and $\alpha-$ and $\beta-BHC$ were $2{\times}10^{-4}$ g and $1.0{\times}10^{-4}$ g respectively.

• Korean Journal of Environmental Agriculture
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• v.16 no.4
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• pp.333-340
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• 1997

An analytical method was developed to determine residues of haloxyfop-R and its methyl ester in soils and soybeans using gas-liquid chromatography (GLC) with electron capture detector (ECD). Soil or soybean sample was acidified and extracted with acetone. The extract was then subjected to ion-associated partition to individually separate haloxyfop-R and the neutral methyl ester. One phase containing haloxyfop-R was methylated with $BF_3$/methanol, partitioned to n-hexane and analyzed by GLC/ECD. The other phase containing the methyl ester was further purified by Florisil column chromatography prior to GLC determination. No cross contamination was found between two phases containing each of the acid and methyl ester, thus two compounds can be separately determined as the identical haloxyfop-R-methyl. Overall recoveries of haloxyfop-R from fortified samples averaged 88.2${\pm}$3.9% (n=12) and 88.3${\pm}$4.0% (n=6) for soils and soybeans respectively, and those of haloxyfop-R-methyl showed mean values of 89.2${\pm}$4.0% (n=12) and 85.6${\pm}$5.6% (n=6). Detection limits of both haloxyfop-R and its methyl esterwere 0.005㎎/㎏ and 0.01㎎/㎏ for soil and soybean samples respectively.

• The Korean Journal of Pesticide Science
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• v.9 no.4
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• pp.292-302
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• 2005

Condition of Ion-Trap gas chromatography-mass spectrometry (GC-MS) for rapid screening of 206-pesticides residues in agricultural foodstuffs was optimized. As applying a wide-bore column (10 m${\times}$0.53 mm, DF 0.25 um) connected with a fused silica restrictor (0.6 m${\times}$0.1 mm), a significant retention time reduction was obtained. Additionally, the shape of peaks was sharper and higher than classical GC's and GC-MS's, which allowed lower detection limits. To easily manage many spectral data, both of Electron Ionization(EI) and Chemical Ionization(CI) techniques were adopted in screening procedure. At the following steps, MS-MS technique were used to confirm screened analytes in complicated matrices.