• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.13-21
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• 2019

A method was developed for the simultaneous detection of an antibiotic fungicide, streptomycin, and its metabolite (dihydrostreptomycin) in agricultural products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted using methanol adjusted to pH 3 using formic acid, and purified with a HLB (Hydrophilic lipophilic balance) cartridge. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.001 to 0.1 mg/kg, and linearity of five agricultural products (hulled rice, potato, soybean, mandarin, green pepper), with coefficients of determination $(R^2){\geq}0.9906$, for streptomycin and dihydrostreptomycin. The mean recoveries at three fortification levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) were from 72.0~116.5% and from 72.1~116.0%, and relative standard deviations were less than 12.3% and 12.5%, respectively. The limits of quantification (LOQ) were 0.01 mg/kg, which are satisfactory for quantification levels corresponding with the Positive List System. All optimized results satisfied the criteria ranges requested in the Codex guidelines and the Food Safety Evaluation Department guidelines. The present study could serve as a reference for the establishment of maximum residue limits and be used as basic data for detection of streptomycin and dihydrostreptomycin in food.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.235-241
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• 2019

An analytical method was developed for the determination of an antibiotic fungicide, kasugamycin, in agricultural products (hulled rice, potato, soybean, mandarin and green pepper) using liquid chromatographytandem mass spectrometry (LC-MS/MS). Samples were extracted with methanol adjusted to pH 13 using 1 N sodium hydroxide, and purified with a HLB (hydrophilic lipophilic balance) cartridge. Linearity of a matrix-matched calibration curve using seven concentration levels, from 0.001 to 0.1 mg/kg, was excellent with a correlation coefficient ($R^2$) of more than 0.9998. The limits of detection (LOD) and quantification (LOQ) of instrument were 0.0005 and $0.001{\mu}g/mL$, respectively, and the LOQ of analytical method calculated as 0.01 mg/kg. The average recoveries at three spiking levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) were in the range of 71.2~95.4% with relative standard deviation of less than 12.1%. The developed method was simple and all optimized results was satisfied with the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. The present study could be served as a reference for the establishment of maximum residue limits (MRL) of kasugamycin and be used as basic data for safety management relative to kasugamycin residues in imported and domestic agricultural products.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.115-123
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• 2019

An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.

• Journal of Food Hygiene and Safety
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• v.39 no.2
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• pp.72-82
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• 2024

This study aimed to develop a scientifically and systematically standardized xylooligosaccharide analytical method that can be applied to products with various formulations. The analysis method was conducted using HPLC with Cadenza C₁₈ column, involving pre-column derivatization with 1-phenyl-3-methyl-5-pyrazoline (PMP) and UV detection at 254 nm. The xylooligosaccharide content was analyzed by converting xylooligosaccharide into xylose through acid hydrolysis. The pre-treated methods were compared and evaluated by varying sonication time, acid hydrolysis time, and concentration. Optimal equipment conditions were achieved with a mobile phase consisting of 20 mM potassium phosphate buffer (pH 6)-acetonitrile (78:22, v/v) through isocratic elution at a flow rate of 0.5 mL/min (254 nm). Furthermore, we validated the advanced standardized analysis method to support the suitability of the proposed analytical procedure such as specificity, linearity, detection limits (LOD), quantitative limits (LOQ), accuracy, and precision. The standardized analysis method is now in use for monitoring relevant health-functional food products available in the market. Our results have demonstrated that the standardized analysis method is expected to enhance the reliability of quality control for healthy functional foods containing xylooligosaccharide.

• Food Science and Preservation
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• v.16 no.6
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• pp.789-796
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• 2009

Benzoic acid (BA) and sorbic acid (SA) are the preservatives most commonly used in food. Although BA and SA are generally safe, some previous studies have shown that consumption of excessive amounts of these food additives can be a health hazard. The aim of this study was to determine the amounts of BA and SA in processed foods in Korea. Different brands of fruit juice, yogurt, cheese, dried fruits, jam, and margarine were purchased at a local market in Daejeon, Korea. Samples were analyzed by high-performance liquid chromatography (HPLC) using a UV detector. Chromatographic separation was achieved with a C18 column. Methanol acetate buffer (pH 4.4) at a 35:65 v/v ratio was used as the initial mobile phase to elute BA and SA. The detector wavelength was set at 254 nm. The average test results observed for BA concentrations in fruit juice, yogurt, cheese, dried fruits, jam, and margarine were $40.26{\pm}0.02$, $2.07{\pm}0.06$, $0.02{\pm}0.09$, $0.36{\pm}08$, $265.30{\pm}0.02$, and $27.34{\pm}0.08\;mg/kg$, respectively. Average concentrations of SA in these samples were $0.92{\pm}0.06$, $1.06{\pm}0.07$, $7.30{\pm}0.01$, $14.14{\pm}0.08$, $25.65{\pm}0.06$, and $4.81{\pm}0.07\;mg/kg$, respectively. Thus, the average levels of BA and SA in the studied food items were lower than the KFDA-permitted limits. Moreover, the estimated daily intake of both BA and SA by a typical consumer were below the maximum recommended daily values.

• Korean Journal of Environmental Agriculture
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• v.38 no.4
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• pp.321-331
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• 2019

BACKGROUND: Pinoxaden is the phenylpyrazoline herbicide developed by Syngenta Crop Protection, Inc. and marketed on 2006. The maximum residue levels for wheat and barley were set by import tolerance. Thus, Ministry of Food and Drug Safety (MFDS) official analytical method determining Pinoxaden residue was necessary in various food matrixes. Satisfaction of international guideline of CODEX (Codex Alimentarius Commission CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) are additional pre-requirements for analytical method. In this study, liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was investigated to analyze residue of Pinoxaden (M4), which is defined as pesticide residue in Korea, in foods. METHODS AND RESULTS: Pinoxaden (M4) was extracted followed by acid digestion (2hr reflux with 1N HCl) and pH adjusting (pH 4-5 with 3% ammonium solution). To remove oil, additional clean-up step with hexane saturated with acetonitrile was required to high oil contained sample before purification. HLB cartridge and nylon syringe filter were used for purification. Then, samples were analyzed by LC-MS/MS using reserve phase column C₁₈. Five agricultural group representative commodities (mandarin, potato, soybean, hulled rice, and red pepper) were used to verify the method in this study. The liner matrix-matched calibration curves were confirmed with coefficient of determination (r²) > 0.99 at calibration range 0.002-0.2 mg/kg. The limits of detection and quantitation were 0.004 and 0.01 mg/kg, respectively, which were suitable to apply Positive List System (PLS). Mean average accuracies of pinoxaden (M4) were shown to be 74.0-105.7%. The precision of pinoxaden and its metabolites were also shown less than 14.5% for all five samples. CONCLUSION: The method investigated in this study was suitable to CODEX (CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

• Journal of Environmental Health Sciences
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• v.41 no.5
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• pp.289-298
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• 2015

Objectives: The method of analyzing urinary arsenic by flow injection hydride generation atomic absorption spectrometry (FI-HG-AAS) is generally used because it shows relatively greater sensitivity, low detection limits, low blocking action, and is simple to operate. In this study, the results of analysis according to three pre-reductants commonly used in the FI-HG-AAS method were compared with each other. Methods: To analyze urinary arsenic, nineteen urine samples were collected from adults aged 43-79 years old without occupational arsenic exposure. Analysis equipment was FI-HG-AAS (AAnalyst 800/FIAS 400, Perkin- Elmer Inc., USA). The three pre-reductants were potassium iodide (KI/AA), C3H7NO2S (L-cysteine), and a mixture of KI/AA and L-cysteine (KI/AA&L-cysteine). Results: In the results of the analysis, the recovery rate of the method using KI/AA was 82.3%, 95.7% for Lcysteine, and 123.5% for KI/AA and L-cysteine combined. When compared with the results by use of high performance liquid chromatography inductively-coupled plasma mass spectrometry (HPLC-ICP-MS), the method using L-cysteine was the closest to those using HPLC-ICP-MS ($98.57{\mu}g/L$ for HPLC-ICP-MS; $74.96{\mu}g/L$ for L-cysteine; $69.23{\mu}g/L$ for KI/AA and L-cysteine; $13.06{\mu}g/L$ for KI/AA) and were significantly correlated (R2=0.882). In addition, they showed the lowest coefficient of variation in the results between two laboratories that applied the same method. Conclusion: The efficiency of hydride generation is considered highly important to the analysis of urinary arsenic via FI-HG-AAS. This study suggests that using L-cysteine as a pre-reductant may be suitable and the most rational among the FI-Hg-AAS methods using pre-reductants.

• Journal of the Korean Geotechnical Society
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• v.29 no.10
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• pp.67-74
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• 2013

The objective of this study was to identify the effect of engineering properties on the resilient modulus ($M_r$) of cohesive soils as subgrade. Eight representative cohesive soils representing A-6, and A-7-6 soil types collected from road construction sites, were tested in the laboratory to determine their basic engineering properties. The laboratory tests for the engineering properties were Atterberg limits test, sieve analysis, hydrometer test, Standard Proctor compaction test, and unconfined compressive strength test. Resilient modulus test and unconfined compressive strength test were conducted on unsaturated cohesive soils at three different moisture contents (dry of optimum moisture content, optimum moisture content, and wet of optimum moisture content). The increase in moisture content considerably affected the decrease in the resilient modulus. The resilient modulus increased with an increase in maximum unconfined compressive strength, percent of clay, percent of silt and clay, liquid limit and plasticity index. The resilient modulus decreased with an increase in percent of sand.

• The Korean Journal of Cytopathology
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• v.12 no.1
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• pp.1-15
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• 2001

The Bethesda System (TBS) was first developed in 1988 for the need to enhance the communication of the cytopathologic findings to the referring physician in unambiguous diagnostic terms. The terminology used in this reporting system should reflect current understanding of the pathogenesis of cervical/vaginal disease so the framework of the reporting system should be flexible enough to accommodate advances in medicine including virology, molecular biology, and pathology. Three years after the Introduction of TBS, the second Bethesda workshop was held to set or amend diagnostic criteria for each categories of TBS. TBS 1991 is now widely used. The third Bethesda workshop, The Bethesda System 2001 Workshop, was held in National Cancer institute Bethesda, Maryland from April 30 to May 2, 2001. Again, the goals of this workshop were to promote effective communication and to clarify in reporting cervical cytopathology results to clinicians and to provide with the information to make appropriate decisions about diagnosis and treatment. Nine forum groups were made and there were Web-based bulletin board discussions between October, 2000 and the first week of April, 2001. On the basis of bulletin board comments and discussions, the forum moderators recommended revised terminologies in the Workshop. Hot discussions were followed after the presentation by forum moderators during the workshop. Terminologies confusing clinicians and providing no additional informations regarding patient management were deleted in the workshop to clarify the cervicovaginal cytology results. Any informations related to the patient management were encouraged to add. So 'Satisfactory for evaluation but limited by...' of 'Specimen Adequacy' catergory was deleted. Terminology of 'Unsatisfactory' was further specified as 'Specimen rejected' and 'Specimen processed and examined, but unsatisfactory'. Terminologies of 'Benign Cellular Change' and 'Within Normal Limits' were combined and terminology was changed to 'Negative for intraepithelial lesion or malignancy'. In General categorization, category 'Other' was newly inserted and the presence of 'Endometrial cells' in women over 40 years old can be checked. Although the category 'Benign Cellular Change' was deleted, the organisms or reactive changes of this category can be listed in the descriptive diagnoses. Terminologies of ASCUS and AGUS were changed to atypical squamous cell and atypical glandular cell, respectively. Diagnostic term of 'Adenocarcinoma in situ', which is highly reproducible with reliable diagnostic criteria, was newly Inserted. The category of hormonal evaluation was deleted. Criteria for liquid-based specimen were discussed. Reporting by computer-assisted cytology was discussed and terminology for automated review was newly inserted. This is not the final edition of Bethesda 2001. The final document can be prepared before the ASCCP meeting in which Consensus Guidelines for the Management on Cytology Abnormalities and Cervical Precursors will develop in September 2001.

• Journal of Food Hygiene and Safety
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• v.28 no.3
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• pp.267-271
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• 2013

A survey of aflatoxin $B_1$ and ochratoxin A was conducted on dried red pepper and red pepper powder. Total number of 193 samples were collected from local markets in Incheon. The presence of aflatoxin $B_1$ and ochratoxin A was determined by high performance liquid chromatography (HPLC) with fluorescence detector using immunoaffinity column clean-up. The recovery rate of aflatoxin $B_1$ and ochratoxin A were more than 80% and the limits of quantification were 0.13 ${\mu}g/kg$ for aflatoxin $B_1$ and 0.30 ${\mu}g/kg$ for ochratoxin A. Aflatoxin $B_1$ was detected in 33 samples (17.1%) with a range of 0.14~9.67 ${\mu}g/kg$ and ochratoxin A was detected in 40 samples (20.7%) with a range of 0.31~3.31 ${\mu}g/kg$. These results show that the occurrence of aflatoxin $B_1$ and ochratoxin A in dried red pepper and red pepper powder tested in this study is low compared with the standard in Korea Food Code (10 ${\mu}g/kg$ as aflatoxin $B_1$ and 7 ${\mu}g/kg$ as ochratoxin A).