• Korean Journal of Veterinary Service
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• v.44 no.3
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• pp.125-131
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• 2021

Benzimidazole is an widely used anthelmintics in livestock clinics. The aim of present study was to investigate benzimidazole residues in the meat in Sejong City. A total of 338 samples of meat(beef 287, pork 37, chicken 14) were selected from the laboratory meat(Korean beef genetic test, hygiene test) supplied to school in Sejong City. Representative benzimidazole class drug such as thiabendazole, 2-amino albendazole sulfone, fenbendazole, oxfendazole, and oxfendazole sulfone were monitored in samples by using lc-ms/ms and the analysis was preformed based on the Korea Food Code guideline. Limit of quantitation (LOQ) was ranged from 0.56 to 3.02 ppb for target drugs and the accuracy was within the acceptance criteria. Among the sample analyzed only one case, the pork meat was found to have drug levels that exceed LOQ. However, the overall residue concentration was 2.17 ppb, which was lower than the maximum residue levels (100 ppb).

• Journal of the Korean Society of Food Science and Nutrition
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• v.45 no.3
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• pp.342-351
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• 2016

This study was carried out to develop an optimized analytical method using high-performance liquid chromatography (HPLC) applied to canthaxanthin, which is not yet designated as a food colorant in Korea, as well as to perform validation and uncertainty evaluation of this method. Official methods of AOAC, UK, and Japan with HPLC-UV detection were evaluated for the analysis of canthaxanthin by comparison of linearity, resolution, selectivity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision, recovery, inter-laboratory tests, and uncertainty measurement. The calibration curves showed high linearity with an $R_2$ value of over 0.999 for canthaxanthin standard solutions in all three official methods. The official method of Japan exhibited the best results in terms of resolution and selectivity, including the lowest LOD and LOQ. The average coefficients of variation were calculated as less than five of three institutes with a precision value less than 1, accuracy near 100%, and recovery ratio between $100{\pm}10%$. The expanded uncertainty for canthaxanthin was estimated to be $39.5{\pm}5.29mg/kg$ (95% confidence level, k=2), and the uncertainty of measurement was 13.4%. In this study, official methods of canthaxanthin were compared and the validities verified. The results will be further applied to establish an authorized analytical method for canthaxanthin in Korea.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.140-147
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• 2019

An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

• Journal of Food Hygiene and Safety
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• v.37 no.4
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• pp.216-224
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• 2022

This study was aimed at validating the analysis methods for deacetylasperulosidic acid (DAA), total sugar, galacturonic acid, glucose, and galactose, which are the indicator components of fermented Morinda citrifolia polysaccharide extract (Vitalbos). We modified the previously reported methods for validating the analytical methods. The specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) were measured using phenol-sulfuric acid method and high-performance liquid chromatography (HPLC). The retention time and spectrum of the standard solution of Vitalbos coincided, confirming the specificity. The calibration curve correlation coefficient (R²), of five indicator components, ranged from 0.9995-0.9998, indicating excellent linearity of 0.99 or more. The intra-day and inter-day precision range of the assay was 0.14-3.01%, indicating a precision of less than 5%. The recovery rate was in the range of 95.13-105.59%, presenting excellent accuracy. The LOD ranged from 0.39 to 0.84 ㎍/mL and the LOQ ranged from 1.18 to 2.55 ㎍/mL. Therefore, the analytical method was validated for DAA, total sugar, galacturonic acid, glucose, and galactose, in Vitalbos. The indicator component content in Vitalbos was determined using a validated method. The contents of DAA, total sugar, galacturonic acid, glucose, and galactose were 2.31±0.06, 475.92±5.95, 72.83±1.05, 71.63±2.44, and 67.30±2.31 mg/g of dry weight, respectively. These results suggest that the developed analytical method is efficient and could contribute to the quality control of Vitalbos, as a healthy functional food material.

• Korean Journal of Oriental Medicine
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• v.11 no.2
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• pp.167-178
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• 2005

As a part of the quality control of herbal prescriptions which has been used for diabetes and related diseases, a reversed-phase liquid chromatographic method was developed for the simultaneous quantification of the three marker compounds, puerarin (Puerariae Radix), glycyrrhizin (Glycyrrhizae Radix), schizandrin (Schizandrae Fructus) in Oc Chun San. The HPLC analysis method was validated for parameters such as linearity, Limits of Detection(LOD), quantification(LOQ), repeatability, stability and recovery.

• Bulletin of the Korean Chemical Society
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• v.32 no.2
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• pp.489-497
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• 2011

The proposed method for an effective assay of Cd, Cr and Pb in several polymer samples has been validated. The determination was carried out using ICP-OES after a high pressure asher (HPA) digestion at pressure and temperatures up to 13 MPa and $320^{\circ}C$, respectively. Polymer based materials were totally oxidized with nitric acid in a HPA chamber and determined by ICP-OES. Validation parameters such as linearity, matrix effect, limit of dectection (LOD), limit of quantitation (LOQ), accuracy and precision (repeatibility, intermediate precision and reproducibility) were assessed. The LOD and LOQ in the sample were ranged from 0.98 to 1.18 mg $kg^{-1}$ and 2.93 to 3.55 mg $kg^{-1}$, respectively, relying on the analyte. The proposed method had a good accuracy and precision for repeatability, intermediate precision with respect to days and analysts and reproducibility expressed as inter-laboratory study. The developed method was simple to use, suitable and applicable to various kinds of polymers.

• Proceedings of the Korea Society of Environmental Toocicology Conference
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• 2004.05a
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• pp.73-73
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• 2004

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.185-194
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• 2015

This study was performed to establish a single residue analytical method for determining fungicide carpropamid residues in various agricultural commodities. Korean cabbage, apple, brown rice and green pepper were selected as representative crops. Samples were homogenized, extracted with acetone and purified by liquid-liquid partition and Florisil column chromatography. Carpropamid residues were analyzed at 220 nm with reversed phase HPLC equipped octylsilyl and octadecylsilyl column and confirmed using mass spectrometry. ILOQ (Instrumental limit of quantitation) of carpropamid was 2 ng and MLOQ (Method LOQ) was 0.02 mg/kg. Mean recoveries from four kinds of crop samples fortified at three levels (MLOQ, 10LOQ, 100LOQ) in triplicate were in the range of 84~112%. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types.

• Journal of Food Hygiene and Safety
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• v.26 no.1
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• pp.12-15
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• 2011

A method based on high-performance liquid chromatography (HPLC) with ultraviolet detection has been developed to quantify coenzyme Q10 (CoQ10) in raw materials and dietary supplements. Single-laboratory validation has been performed on the method to determine linearity, selectivity, accuracy, limits of quantification (LOQ) and repeatability for CoQ10. An excellent linearity (r=0.999) was observed for CoQ10 in the concentration range $15.625{\sim}500\;{\mu}g/ml$ in dietary supplement. Observed recovery of CoQ10 was found to be between 98.33 and 99.38%. LOQ was found to be $250\;{\mu}g/ml$ Repeatability precision for CoQ10 was between 0.15 and 0.21% relative standard deviation (RSD). Further, limited studies showed that some adulterants and degraded material could be satisfactorily separated from CoQ10 and identified.

• Korean Journal of Environmental Agriculture
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• v.33 no.3
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• pp.213-219
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• 2014

BACKGROUND: In an environment-friendly agriculture, plant extracts have been perceived as alternatives of synthetic pesticides. The Environment-friendly Agriculture Promotion Act of Korea has approved cinnamon extract as a matter for the production of commercial biopesticides. Thirteen commercial biopesticides containing cinnamon extract have been marketed locally. However, the analytical method for the quality control of these biopesticides containing cinnamon extract has not been studied. METHODS AND RESULTS: Cartridge clean-up method for the determination of cinnamaldehyde, cinnamylalcohol and salicylaldehyde in biopesticides containing cinnamon extract was developed and validated by gas chromatography (GC). The clean-up method was optimized with HLB SPE cartridges for the bioactive substance in biopesticides containing cinnamon extract, and the eluate was analyzed by GC. The developed method was validated, and the LOQ and recovery rates of cinnamaldehyde, cinnamylalcohol and salicylaldehyde were 0.139, 0.067 and $0.062mgL^{-1}$ and 84.2, 86.5 and 82.1%, respectively. The contents of cinnamaldehyde, cinnamylalcohol and salicylaldehyde were analyzed using the developed method in the 13 commercial biopesticides. Results showed 0.06-17.37%,