• Journal of Food Hygiene and Safety
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• v.32 no.5
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• pp.381-388
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• 2017

In this study, we investigated the levels of natural preservatives of benzoic acid, sorbic acid, and propionic acid in spices. The quantitative analysis was performed using high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) for benzoic acid and sorbic acid and gas chromatography-mass spectrometry (GC-MS) for propionic acid. The sample was extracted with ethanol using sonication, then centrifuged and evaporated to dryness and redissolved to 1 mL with ethanol to use for the instrumental analysis. The analytical method was validated based on linearity, recovery, limit of detection (LOD), and limit of quantification (LOQ). This method was suitable to determine low amounts of naturally occurring preservatives (benzoic acid, sorbic acid, and propionic acid) in various spices. Benzoic acid, sorbic acid, and propionic acid were found in 165 samples, 88 samples, and 398 samples, respectively from the total of 493 samples. The concentration of benzoic acid, sorbic acid, and propionic acid were ranged at ND-391.99 mg/L, ND-57.70 mg/L, and ND-188.21 mg/L in spices, respectively. The highest mean levels of benzoic acid, sorbic acid, and propionic acid were found in cinnamon (167.15 mg/L), basil leaves (22.79 mg/L), and white pepper (51.48 mg/L), respectively. The results in this study provide ranges of concentration regarding naturally occurring benzoic acid, sorbic acid, and propionic acid in spices. Moreover, the results may use to the case of consumer complaint or trade friction due to the inspection services of standard criteria for the preservatives of spices.

• Journal of Food Hygiene and Safety
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• v.32 no.4
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• pp.298-305
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• 2017

Benzovindiflupyr is a new pyrazole carboxamide fungicide that inhibits succinate dehydrogenase of mitochondrial respiratory chain. This study was carried out to develop an analytical method for the determination of benzovindiflupyr residues in agricultural commodities using LC-MS/MS. The benzovindiflupyr residues in samples were extracted by using acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient ($r^2$) of benzovindiflupyr standard solution was 0.99 over the calibration ranges ($0.001{\sim}0.5{\mu}g/mL$). Recovery tests were conducted on 5 representative agricultural commodities (mandarin, green pepper, potato, soybean, and hulled rice) to validate the analytical method. The recoveries ranged from 79.3% to 110.0% and then relative standard deviation (RSD) was less than 9.1%. Also the limit of detection (LOD) and limit of quantification (LOQ) were 0.0005 and 0.005 mg/kg, respectively. The recoveries of interlaboratory validation ranged from 83.4% to 117.3% and the coefficient of variation (CV) was 9.0%. All results were followed with Codex guideline (CAC/GL 40) and Ministry of Food and Safety guideline (MFDS, 2016). The proposed new analytical method proved to be accurate, effective, and sensitive for benzovindiflupyr determination and would be used as an official analytical method.

• Journal of Food Hygiene and Safety
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• v.32 no.4
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• pp.329-335
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• 2017

Analysis method was presented for the simultaneous determination of nine bisphenol A related compounds such as bisphenol A (BPA), phenol, p-tert-butylphenol, bisphenol A diglycidyl ether (BADGE), $BADGE{\cdot}2H_2O$, $BADGE{\cdot}2HCl$, bisphenol F diglycidyl ether (BFDGE), $BFDGE{\cdot}2H_2O$ and $BFDGE{\cdot}2HCl$ migrated from inner coatings of metal food cans by high performance liquid chromatography (HPLC) with fluorescence detection. The method was validated by examining the linearity of calibration curve, the limit of detection (LOD), the limit of quantification (LOQ), recovery and uncertainty. The migration tests of nine BPA related compounds were carried out with four food simulants; deionized water (DW), 4% acetic acid, 50% ethanol and n-heptane. There was not any compound detected in DW, 4% acetic acid and 50% ethanol at $60^{\circ}C$ for 30 min and n-heptane at $25^{\circ}C$ for 60 min. BPA and phenol were migrated into 4% acetic acid and 50% ethanol at $95^{\circ}C$ for 30 min. The concentrations were ranged from 0 to $10.77{\mu}g/L$ of BPA and from 0 to $2.35{\mu}g/L$ of phenol. Canned foodstuffs mostly have long-term shelf life. We investigated migration of nine BPA related compounds according to the variation in storage periods (0~90 days) and temperatures (4, 25 and $60^{\circ}C$). All compounds were not founded during 90 days at $4^{\circ}C$ and $25^{\circ}C$, respectively. However BPA and $BADGE{\cdot}2H_2O$ were founded in DW and 4% acetic acid at $60^{\circ}C$. The migration levels of BPA and $BADGE{\cdot}2H_2O$ were close to the value of LOQ, respectively and did not change significantly as storage period. It was founded from results that the migration of BPA related compounds from metal food cans was controlled to a safe level.

• Korean Journal of Food Science and Technology
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• v.42 no.1
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• pp.1-7
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• 2010

To revise the dithiocarbamates residue analysis method and survey the residues in agricultural products that were treated with these fungicides in Korea, we purchased 20 types of foodstuffs (rice, potato, cabbage, apple etc.) from markets in five major cities. 236 samples of the purchased foodstuffs were then analyzed for the presence of dithiocarbamates by HPLC/UV and HPLC/APCI-MS. The $R^2$, LOD and LOQ in the range of 0.5-107.3 mg/L were as follows: DCC: y=174.34x+18.315, $R^2=0.9999$, 0.01 mg/L, and 0.04 mg/L; EBDC: y=227.38x-14.715, $R^2=1.0000$, 0.01 mg/L and 0.02 mg/L; PBDC: y=38.46x-21.412, $R^2=0.9999$, 0.04 mg/L, and 0.1 mg/L; ETU: y=52.752x-4.4819, $R^2=0.9998$, 0.02 mg/L and 0.03 mg/L; PTU: y=128.28x+4.4624, $R^2=0.9998$, 0.02 mg/L, and 0.04 mg/L. The levels of DDC, EBDC, PBDC, ETU and PTU in 20 agricultural products fortified to 10.0-107.3 mg/L ranged from 61.7-117.5%, 65.3-110.1%, 61.5-109.6%, 69.3-116.3% and 70.2-97.2%, respectively. Overall, dithiocarbamates were detected in 100 samples and the detection ratio was 42.4%. Among these, only 3 samples (1.3%) of Lycii fructus had residue levels that were above the action limits, while the remaining samples (233 samples) contained levels of dithiocarbamates below the detection limit or below the Korea MRLs (Maximum Residue Limits).

• Korean Journal of Environmental Agriculture
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• v.34 no.4
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• pp.336-344
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• 2015

BACKGROUND: This study was carried out to collect occurrence data on aluminum in 12 type agricultural products and assess dietary exposure risk to the Korean population health for aluminum concentration in agricultural products.METHODS AND RESULTS: Aluminum analysis samples were performed using microwave device and Inductively Coupled Plasma Optical Emission Spectrometer. The LOD(Limit of Detection) for aluminum was 0.851 μg/kg, while the LOQ(Limit of Quantitation) was 2.838 μg/kg and recovery was 97.6% for aluminum. The average levels of aluminum in mg/kg were 0.526 for rice, 0.546 for Korean cabbage, 1.316 for corn, 6.207 for soybean, 0.549 for sweet potato, 0.257 for potato, 6.963 for spinach, 1.213 for carrot, 0.524 for garlic, 0.950 for radish, 1.015 for leek, and 3.511 for Welsh onion. The dietary exposures of aluminum through usual intake were polished rice 89.31 μg/day, Korean cabbage 33.14 μg/day, corn 0.66 μg/day, soybean 3.72 μg/day, sweet potato 6.86 μg/day, potato 4.96 μg/day, spinach 45.96 μg/day, carrot 6.79 μg/day, garlic 2.36 μ g/day, radish 7.32 μg/day, leek 2.23 μg/day and Welsh onion 43.89 μg/day, taking 0.57%, 0.21%, 0.00%, 0.02%, 0.04%, 0.03%, 0.04%, 0.04%, 0.02%, 0.05%, 0.01% and 0.28% of PTWI(2 mg/kg b.w./week), respectively.CONCLUSION: The levels of overall dietary exposure to aluminum for Korean population through intake of agricultural product was far below the recommended JECFA level, indicating of least possibility of risk.

• Journal of Food Hygiene and Safety
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• v.35 no.1
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• pp.23-30
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• 2020

This study investigated the migration levels of lead (Pb), cadmium (Cd), and arsenic (As) from food contact articles (glassware, ceramics, enamelware, and earthenware) into a food stimulant (4% v/v, acetic acid). Migration tests were performed at 25℃ for 24 h and all analyses were performed using Inductively-Coupled Plasma Mass Spectrometry (ICP-MS). The method was validated by linearity of calibration curves, limit of detection (LOD), limit of quantification (LOQ), recovery, precision, and uncertainty. In glassware, the migration concentrations ranged from not-detected (N.D.) to 752.21 ㎍/L and N.D. to 1.99 ㎍/L for Pb and Cd, respectively. In ceramics, the migration concentrations ranged from N.D. to 1,955.86 ㎍/L, N.D. to 74.06 ㎍/L, and N.D. to 302.40 ㎍/L for Pb, Cd, and As, respectively. In enamelware, the migration concentrations ranged from N.D. to 4.48 ㎍/L, N.D. to 7.00 ㎍/L, and N.D. to 52.00 ㎍/L for Pb, Cd, and Sb, respectively. In earthenware, the migration concentrations ranged from N.D. to 13.68 ㎍/L, N.D. to 0.04 ㎍/L, and N.D. to 6.71 ㎍/L for Pb, Cd, and As, respectively. All results were below the migration limits of Korea standards and specifications for food utensils, containers, and packages.

• Journal of Food Hygiene and Safety
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• v.35 no.4
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• pp.365-374
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• 2020

This study was conducted to monitor the residual pesticides on a total of 320 stalk and stem vegetables from January 2019 to December 2019 in the Incheon metropolitan area. Pesticide residues in samples were analyzed by the multi-residue method for 373 pesticides using GC-MS/MS, LC-MS/MS, GC-ECD, GC-NPD and HPLC-UVD. Risk assessment was also carried out based on the amount of stalk and stem vegetables consumed. The linearity correlation coefficient for the calibration curve was 0.9951 to 1.0000, LOD 0.002 to 0.022 mg/kg, LOQ 0.005 to 0.066 mg/kg and recovery was 82.0 to 108.0%. According to the monitoring of pesticides, 36 (11.3%) of 320 were detected with pesticide residues and 3 (0.9%) samples exceeded the maximum residual limit. The detection frequency for Chinese chives and Welsh onion was higher than that for other stalk and stem vegetables. The frequently detected pesticides were etofenprox, procymidone, fludioxonil, and pendimethalin. As a tool of risk assessment through the consumption of pesticide detectable agricultural products, the ratio of estimated daily intake (EDI) to acceptable daily intake (ADI) was calculated in the range of 0.0062-24.1423%. These results indicate that there is no particular health risk through consumption of commercial stalk and stem vegetables detected with pesticide residues.

• Journal of Life Science
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• v.24 no.3
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• pp.252-259
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• 2014

The leaves of Peatasites japonicus are a traditional oriental medicine with diverse biological activities. A simple and specific analytical method for the quantitative determination of bakkenolide B constituents from methanolic extract of the leaves of P. japonicus was developed. Bakkenolide B was isolated from the leaves of P. japonicus, and its structure was elucidated based on 1D, 2D NMR, and GC-MS spectral data. A liquid chromatographic method was developed to evaluate the quality of P. japonicus through determination of major active compound, bakkenolide B. The wavelengths at 254 and 215 nm were chosen to determine bakkenolide B. The recovery of the method was in the range of 98.6 to 103.1%, and bakkenolide B showed good linearity ($r^2$=0.999) within test ranges. The developed method was applied to the determination of bakkenolide B in the plant part and seasonal changes. The results showed that the content of bakkenolide B in the leaf was higher than in the petiole and rhizome. In this study, a simple, rapid, and reliable high-performance liquid chromatography method was used to determine the percentage and composition of bakkenolide B in P. japonicus procured from different Petasites species plants in South Korea. The method can be employed in routine quantitative analysis and quality control of different products in the market.

• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.463-470
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• 2011

This study was carried out to survey the residual characteristic of chlorpyrifos and estimate their residues in squash before harvest. The pesticide was sprayed onto the crop at the recommended and its double rates 10 days before the prearranged harvest and sampling was done at 0, 2, 3, 5, 6, 7 and 10 days after spraying. The amounts of the chlorpyrifos residue in the crop was analyzed by chromatographic method. Limit of detection (LOD) of chlorpyrifos was 0.005 mg/kg and its recovery ranged from 95.21 to 102.69%. The initial concentration of chlorpyrifos sprayed with recommended dose exceeded its MRL of 0.1 mg/kg but its concentration was less than its MRL 10 days after application. However its concentration in case of the double dose was over its MRL both immediately and 10 days after application. Biological half-lives of chlorpyrifos sprayed onto squash was 2.5 and 2.9 days at the recommended and double doses, respectively. Ten days later, the residual concentration of chlorpyrifos in squash was decreased substantially. The concentration of chlorpyrifos was estimated in squash at the given day using its regression equations. The estimated concentration of chlorpyrifos in case of application with recommended dose was below its MRL at 10 days after application but its concentration in case of application with double dose was over its MRL at 10 days of the prearranged harvest. The rate of the estimated daily intake (EDI) of chlorpyrifos to its acceptable daily intake (ADI) was 282% right after application but it decreased to less than 18% at 10 days of the prearranged harvest.

• Journal of agricultural medicine and community health
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• v.29 no.2
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• pp.303-314
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• 2004

Objectives: This study was carried out to assess exposure levels of organic dusts and ammonia in poultry farms in Korea. Methods: A total of six poultry farms were investigated. The farms were located in Namwon, Chonlabuk-do and in Kae-San, Chungchongbuk-do. This study consisted of a questionnaire and measuring organic dusts and ammonia. The questionnaire included the characteristics of the farms, work patterns and the tasks of the poultry farms. Results and Conclusions: The farmers raised the chickens 45 times a year and the average number of years in the poultry farm were eight years ranging from 2 to 12 years. They worked for seven days per week and the average hours spent caring the chickens are 6.3 hours per day. The duration of staying in the confinement buildings was 3.3 hours per day. The work time in summer was longest. The feed and the water supply systems were automatic and the control of ventilation windows used "winch curtain" was semiautomatic. They used mechanical ventilation system in winter and used dilution ventilation system in the other seasons. The geometric mean concentration of total and respirable dust sampled in the poultry confinement buildings was 4.0 mg/$m^3$and 0.9 mg/$m^3$ respectively. The ratio of respirable to total dusts range from 9 to 49 percent. There was no sample exceeding the criteria 10 mg/$m^3$ for total dust and 3 mg/$m^3$ for respirable dust in farms. The criteria have been recommended by Korean Ministry of Labor and American Conference of Governmental Industrial Hygienist. The personal respirable dusts measured during a circle work averaged geometric mean concentration 1.4 mg/$m^3$ Two personal samples were exceeded the threshold 3 mg/$m^3$. There was a positive relation between an index and the personal samples of respirable dusts($R^2$=0.98). The index is calculated by multipling the total number of chickens in the farm by the age of the chickens and then dividing by the volume of the confinement building. The geometric mean concentration of area and personal ammonia samples was 23.3 ppm and 22.2 ppm, respectively. Some of the ammonia samples, both area and personal samples, exceeded the short term exposure limit value 35 ppm.