• Analytical Science and Technology
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• v.29 no.2
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• pp.94-103
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• 2016

An analytical method was developed to determine the amount of spinetoram (spinetoram J and spinetoram L) in livestock samples. The spinetoram was extracted with acetonitrile and purified through a primary secondary amine (PSA) sorbent. The spinetoram residues were then quantified and confirmed using a liquid chromatography–tandem mass spectrometer (LC-MS/MS) in the positive ion mode using multiple reactions monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/kg) into a blank extract with r² > 0.994. The limits of detection and quantification were 0.002 and 0.01 mg/kg, respectively. The recovery results of spinetram ranged between 81.9-106.4% at different concentration levels (LOQ, 10LOQ, 50LOQ, n=5) with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003). An interlaboratory study was conducted to validate the method. The proposed analytical method proved to be accurate, effective, and sensitive for spinetoram determination. The method will be used as an official analytical method in Korea.

• Journal of Korean Society of Environmental Engineers
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• v.27 no.6
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• pp.590-598
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• 2005

An adequate method to identify chromium separation, Cr(III) and Cr(VI), in water samples were studied by using High Performance Liquid Chromatography(HPLC) coupled with Inductively Coupled Plasma Mass Spectometer(ICP-MS) equipped with Dynamic Reaction Cell(DRC). The characteristic distribution of Cr(III) and Cr(VI) in the raw water taken at the six water intake stations in Seoul, was analyzed by the method developed by the authors. The chromium species separated by HPLC was isocratically conducted by using tetrabutylammonium phosphate monobasic(1.0 mM TBAP), ethylenediaminetetraacetic acid(0.6 mM EDTA) and 2% v/v methanol as the mobile phase. 5% v/v methanol was used as flushing solvent. A reactive ammonia($NH_3$) gas was used to eliminate the potential interference of $ArC^+$. Several Parameters such as solvent ratio, pH, flow rate and sample injection volume were optimized for the successful separation and reproducibility. Although it has been reported thai the separation sensitivity of Cr(III) is superior to that of Cr(VI), the authors observed Cr(VI) was more sensitive than Cr(III) when ammonia($NH_3$) gas was used as the reaction gas. It took less than 3 minutes to analyze chromium species with this method and the estimated detection limits were $0.061\;{\mu}g/L$ for Cr(III) and $0.052\;{\mu}g/L$, for Cr(VI). According to the results from the analysis on chromium species in the raw water of the six intake stations, the concentrations of Cr(III) ranged from 0.048 to $0.064\;{\mu}g/L$(ave. $0.054\;{\mu}g/L$) while that of Cr(VI) ranged from 0.014 to $0.023\;{\mu}g/L$(ave. $0.019\;{\mu}g/L$). Recovery ratio was very high($90.1{\sim}94.1%$). There were two or three times more Cr(III) than Cr(VI) in the raw water.

• The Korean Journal of Pesticide Science
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• v.13 no.3
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• pp.190-196
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• 2009

The residues of abamectin 1.8% EC, resisted for control of pine wood nematode, Bursaphelenchus xylophilus in pine tree were surveyed in tissue of Pinus thunbergii and P. koraiensis after injection of a liquid formulation. Limits of detection of abamectin in tissue of P. thunbergii were $0.05\;mg\;kg^{-1}$ and mean recoveries at $0.5\;mg\;kg^{-1}$ trunk injection were 90.9% and 93.1% respectively in stem and trunk of P. thunbergii. Abamectin 1.8% EC, trunk injected in 15 m height P. thunbergii were detected in all stem (edible part of carrier insect of pine wood nematode, Monochamus alternatus) from 0.29 to $0.73\;mg\;kg^{-1}$ after 150 days injection. Amount of residue of abamectin 1.8% EC in 12.6 cm mean breast height diameter (DBH) P. thunbergii were variable depending on individual trees in natural forest. Amount of residues in lower and middle part of trunk were reduced with the passage of the injection time. In upper part of trunk were detected $1.84\;mg\;kg^{-1}$ on 30 days after injection however $0.65\;mg\;kg^{-1}$ on 15 days after injection and under detection limit on 100 and 180 days after injection in P. thunbergii. Bottom and middle parts of crown were detected $0.183\;mg\;kg^{-1}$ and $0.173\;mg\;kg^{-1}$ respectively on 180 days after injection in P. thunbergii. Mean residues of abamectin in crown and trunk were $0.80\;mg\;kg^{-1}$ and $0.30\;mg\;kg^{-1}$ on 170 days after trunk injection in 20 cm DBH and 9 m height P. koraiensis. Mean residues of abamectin in crown and trunk were $0.67\;mg\;kg^{-1}$ and $0.36\;mg\;kg^{-1}$ on 170 days after trunk injection in 15 cm DBH and 6 m height P. koraiensis.

• Korean Journal of Agricultural Science
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• v.4 no.2
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• pp.157-166
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• 1977

These experiments were carried out to analyse the correlation among various soil parameters which characterize the mechanical properties of the disturbed and undisturbed soil, and to analyse Atterberg Limits for the basin of downstream of Hanriver Keum river, Nakdong river, and Asan bay. 1. Wet density of soil was the lowest in the basin of Nakdong river which contains the highest amount of clay minerals among the soil samples, and was increased in the order of Han river, Keum river and Asan bay. It was appeared that the unit weight of natural soil was changed in accordance with the clay mineral content which determines the moisture content. 2. Curved relationship was recognized, showing that dry density of soil was decreased with increasing the moisture content. Soils from the basin of Asan bay were appeared to have the highest dry density and the next was those of Keum river, the second lowest Han river, and the lowest Nakdong river. 3. When the liquid limit of soils was over 40 percent, their plastic index was above the A-line of plastic chart. 4. Between dry density and void ratio of soils, a curved relationship was found, in which dry density was decreased as void ratio increased, and the differences between them became greater in soils containing higher amount of coarse grained soil. Decreasing tendency of dry density in accordance with increase of void ratio was the most significant at Asan bay which contained the lowest clay content, and other decreasing order of dry density was Keum river, Han river, and Nakdong river.

• Journal of Food Hygiene and Safety
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• v.26 no.2
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• pp.142-149
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• 2011

An isocratic high performance liquid chromatography (HPLC) method for routine analysis of deoxynivalenol in noodles was validated and estimated the measurement uncertainty. Noodles (dried noodle and ramyeon) were analyzed by HPLC-ultraviolet detection using immunoaffinity column for clean-up. The limits of detection (LOD) and quantification (LOQ) were 7.5 ${\mu}g$/kg and 18.8 ${\mu}g$/kg, respectively. The calibration curve showed a good linearity, with correlation coefficients $r^2$ of 0.9999 in the concentration range from 20 to 500 ${\mu}g$/kg. Recoveries and Repeatabilities expressed as coefficients of variation (CV) spiked with 200 and 500 ${\mu}g$/kg were $82{\pm}2.7%$ and $87{\pm}1.3%$% in dried noodle, and $97{\pm}1.6%$ and $91{\pm}12.0%$ in ramyeon, respectively. The uncertainty sources in measurement process were identified as sample weight, final volume, and sample concentration in extraction volume as well as components such as standard stock solution, working standard solution, 5 standard solutions, calibration curve, matrix, and instrument. Deoxynivalenol concentration and expanded uncertainty in two matrixes spiked with 200 ${\mu}g$/kg and 500 ${\mu}g$/kg were estimated to be $163.8{\pm}52.1$ and $435.2{\pm}91.6\;{\mu}g$/kg for dried noodle, and $194.3{\pm}33.0$ and $453.2{\pm}91.1\;{\mu}g$/kg for ramyeon using a coverage factor of two which gives a level of statistical confidence with approximately 95%. The most influential component among uncertainty sources was the recovery of matrix, followed by calibration curve.

• Journal of Food Hygiene and Safety
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• v.32 no.4
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• pp.290-297
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• 2017

The purpose of this study was developed for the determination of tridemorph in agricultural commodities samples. Tridemorph residues in samples were extracted with acetonitrile, partitioned with saline water, and then purified using and aminopropyl ($NH_2$) SPE catridge. The purified samples were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~2.5 ng) into a blank extract with $r^2$ > 0.999. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. The average recovery ranged between 75.9% and 103.7% at different concentration levels (LOQ, 10 LOQ, 50 LOQ, n = 5) with relative standard deviations (RSDs) less than 9.0%. An interlaboratory study was conducted to validate the method by Korea Advanced Food Research Institute. The average recovery ranged between 87.0% and 109.2% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n = 5) with relative standard deviations (RSDs) less than 8.0%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003) and Food Safety Evaluation Department guidelines (2016). The results prove that the developed analytical methods is accurate, effective and sensitive for tridemorph determination.

• Journal of the Korean Geotechnical Society
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• v.15 no.2
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• pp.43-71
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• 1999

This research is an experimental work of developing a construction material using municipal wastewater sludge as liner and cover materials for waste disposal landfill. Weathered granite soil and flyash, produced as a by-product in the power plant, were used as the primary additives to improve geotechnical engineering properties of sludge. For secondary additives, bentonite and cement were mixed with sludge to decrease the permeability and to increase the shear strength, respectively. Various laboratory test required to evaluate the design criteria for liner and cover materials, were carried out by changing the mixing ratio of sludge with the additives. Basic soil properties such as specific gravity, grain size distribution, liquid and plastic limits were measured to analyze their effects on permeability, compaction, compressibility and shear strength properties of mixtures. Laboratory compaction tests were conducted to find the maximum dry densities and the optimum moisture contents of mixtures, and their effectiveness of compaction in field was consequently evaluated. Permeability tests of variable heads with compacted samples, and the stress-controlled consolidation tests with measuring permeabilities of samples during consolidation process were performed to obtain permeability, and to find the compressibility as well as consolidational coefficients of mixtures, respectively. To evaluate the long term stability of sludges, creep tests were also conducted in parallel with permeability tests of variable heads. On the other hand, for the compacted sludge decomposed for a month, permeability tests were carried out to investigate the effect of decomposition of organic matters in sludges on its permeability. Direct shear tests were performed to evaluate the shear strength parameters of mixed sludge with weathered granite, flyash and bentonite. For the mixture of sludge with cement, unconfined compression tests were carried out to find their strength with varying mixing ratio and curing time. On the other hand, CBR tests for compacted specimen were also conducted to evaluate the trafficability of mixtures. Various test results with mixtures were assessed to evaluate whether their properties meet the requirements as liner and cover materials in waste disposal landfill.

• Korean Journal of Poultry Science
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• v.43 no.2
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• pp.111-118
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• 2016

Mycotoxins are secondary metabolites produced by molds, such as Aspergillus, Fusarium and Penicillium, that have adverse effects on animals and humans. Aflatoxin, ochratoxin, zearalenone, fumonisin and deoxynivalenol are the mycotoxins of greatest agro-economic importance and cause acute disease called mycotoxicoses. Mycotoxicosis in poultry birds results in decreased meat/egg production, immunosuppressant, and hepatotoxicosis. Some of toxins or their metabolites may be retained in animal or human tissues and induce health problems. This study was designed to develop a sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the simultaneous detection and quantification of mycotoxins, such as aflatoxin $B_1$, aflatoxin $M_1$, ochratoxin A, zearalenone, fumonisin B and deoxynivalenol, in chicken liver and kidney tissues. The mycotoxins were extracted and purified using modified QUECHERS methods, separated by LC and detected by an electrospray ionisation interface (ESI) and tandem MS. Good precision and linearity were observed for most of six mycotoxins. The recovery test for each mycotoxin in liver and kidney tissues mostly indicated good average recovery rates between 80.94% and 98.10% and the coefficient of variation mostly under 13.78%, except for aflatoxin $M_1$ and fumonisin $B_1$. The limit of detection (LOD) for six mycotoxins was $7.6{\sim}145.79{\mu}g/kg$ in liver tissues and $6.07{\sim}197.20{\mu}g/kg$ in kidney tissues. The quantification limits (LOQ) for 6 mycotoxins were in the range $23.04{\sim}441.78{\mu}g/kg$ in liver tissues and $18.40{\sim}597.59{\mu}g/kg$ in kidney tissues, respectively. The developed multi-mycotoxin method in this study permits simultaneous, simple, and rapid determination of several co-existing mycotoxins in chicken liver and kidney tissues.

• Korean Journal of Environmental Agriculture
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• v.37 no.4
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• pp.283-290
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• 2018

BACKGROUND: Pesticide residue analysis is an essential activity in order to establish the food safety of agricultural products. Analytical approaches to the food safety are required to meet internationally the guideline of Codex (Codex Alimentarius Commission, CAC/GL 40). In this study, we developed a liquid chromatograph-tandem mass spectrometer (LC-MS/MS) method to determine the herbicide clopyralid in food matrixes. METHODS AND RESULTS: Clopyralid was extracted with aqueous acetonitrile containing formic acid and the extracts were mixed in a citrate buffer consisted of magnesium sulfate anhydrous, NaCl, sodium citrate dihydrate and disodium hydrogencitrate sesquihydrate followed by centrifugation. The supernatants were filtered through a nylon membrane filter and used for the analysis of clopyralid. The method was validated by accuracy and precision experiments on the samples fortified at 3 different levels of clopyralid. LC-MS/MS in positive mode was employed to quantitatively determine clopyralid in the food samples. Matrix-matched calibration curves were inearranged from 0.001 to 0.25 mg/kg with r2 > 0.994. The limits of detection and quantification were determined to be 0.001 and 0.01 mg/kg, respectively. There covery values of clopyralid for tified at 0.01 mg/kg in the control samples ranged from approximately 82 to 106% with relative standard deviations below 2 0%. CONCLUSION: The method developed in this study meets successfully the Codex guideline for pesticide residue analysis in food samples. This, the method could be applicable to determine pesticides in foods produced domestically and internationally.

• Journal of Food Hygiene and Safety
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• v.36 no.4
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• pp.298-309
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• 2021

In this study we sought to develop a simultaneous analysis method for cis-bixin and cis-norbixin, the main components, to detect annatto pigment in food. To establish the optimal test method, the HPLC analysis methods of the European Food Safety Authority (EFSA), Japan's Ministry of Health, Labor and Welfare (MHLW), and National Institute of Food and Drug Safety Evaluation (NIFDS) were compared and reviewed. In addition, a new pretreatment method applicable to various foods was developed after selecting conditions for simultaneous high-performance liquid chromatography (HPLC) analysis in consideration of linearity, limit of detection (LOD), limit of quantification (LOQ), and analysis time. The HPLC analysis method of NIFDS showed the best linearity (R² ≥ 0.999), exhibiting low detection and quantification limits for cis-norbixin and cis-bixin as 0.03, 0.05 ㎍/mL, and 0.097, 0.16 ㎍/mL, respectively. All previously reported pretreatment methods had limitations in various food applications. However, the new pretreatment method showed a high recovery rate for all three main food groups of fish meat and meat products, processed cheese and beverages. This method showed an excellent simultaneous recovery rate of 98% or more for cis-bixin and cis-norbixin. The HPLC analysis method with a new pretreatment method showed high linearity with a coefficient of determination (R²) of 1 for both substances, and the accuracy (recovery rate) and precision (%RSD) were 98% and between 0.4-7.9, respectively. From this result, the optimized analytical method was considered to be very suitable for the simultaneous analysis of cis-bixin and cis-norbixin, two main components of annatto pigment in food.