• Journal of Food Hygiene and Safety
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• v.35 no.3
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• pp.243-251
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• 2020

In this study, we investigated pesticide residues in 207 agricultural products distributed by direct trade in the northern area of Gyeonggi Province. A total of 94 general agricultural products and 113 eco-friendly agricultural products collected from local grocers and cooperative stores were analyzed by multiresidue method for 263 pesticides using GC (gas chromatography)/ECD (electron capture detector), GC/NPD (nitrogen phosphorus detector), GC-MS/MS (tandem mass spectrometry), LC (liquid chromatography)/PDA (photodiode array detector), LC/FLD (fluorescence detector), LC-MS/MS. All samples showing pesticide residues were general agricultural products collected from local food stores. The pesticide residue levels of 14 samples (6.8%) were below the maximum residue limits (MRLs) and one of them (0.5%) exceeded the MRLs. Sixteen pesticides were detected from samples of the following produce items: spinach, young cabbage, perilla leaves, mallow, cucumber, chives and water dropwort. The safety of the detected pesticides was assessed by monitoring the daily intake estimate (EDI) and the daily intake allowance (ADI) based on the amount of pesticides detected. The ADI percentage range (the ratio of EDI to ADI) was 0.0134-61.6259% and there was no health risk connected with consuming agricultural products in which pesticide residues were detected.

• The Korean Journal of Pesticide Science
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• v.16 no.3
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• pp.195-201
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• 2012

We tested for pesticide residues in 124 samples of 22 different items of imported fruits circulated in Gyeonggido. Total 218 pesticides were analyzed by multi-residue method using gas chromatography/nitrogen phosphorus detector-electron capture detector (GC/NPD-ECD), time of flight/mass spectrometer (TOF/MS), ultra performance liquid chromatography/photo diode array (UPLC/PDA), high performance liquid chromatography/fluorescence detector (HPLC/FLD) and mass spectrometer (LC/MS/MS). The pesticides were detected in 18 fruits samples, ranging 0.003~0.3 mg/kg and no samples had violative residue. The separation test to 14 sample pesticides detected was conducted to monitor the current status of pesticide residues according to the partial characteristic. The pesticides were detected in 14 peels ranging 0.03~1.5 mg/kg and 2 fleshes in less than detection limits. These results indicate that imported fruits are safe when the human takes normally but even the small amount of pesticides is harmful when the human takes it in a prolonged period. Therefore, the pesticide residual amounts of imported friuts should be constantly monitored for food safety.

• Microbiology and Biotechnology Letters
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• v.27 no.6
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• pp.446-451
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• 1999

The protease produced by Mucor racemosus f. racemosus PDA 103 from meju was purified by precipitating with 80% saturated ammonium sulfate, CM Sephadex C-50 ion-exchange chromatography, and secondary Sephadex G-100 gel filtration chromatography. The specific activity of the purified enzyme was 60.1unit/mg protein and the purification fold of the enzyme was 83.5. The molecular weight of the enzyme was estimated 33,746Da and the enzyme was elucidated as monomer by LC-MS and SDS-PAGE. The number of amino acids was evaluated about 330 residues.

• Journal of Food Hygiene and Safety
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• v.29 no.2
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• pp.92-98
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• 2014

The safety of fake anti-impotence drugs (fake Viagra : 26 samples, fake Cialis : 25 samples) distributed in Gyeonggi province was studied by monitoring the concentrations of anti-impotence pharmaceutical ingredient and their analogues. The concentrations of anti-impotence pharmaceutical ingredient 4 specis and their analogues 17 specis were estimated using by HPLC/PDA, LC-MS/MS. The range of concentration of sildenafil in fake viagra was 40~199 mg/tablet, among them the portion of the concentrations of sildenafil over 150 mg/tablet exceeded 65%. 3 cases in tested samples contained sildenafil and tadalafil. The range of concentration of sildenafil in fake cialis was 102~249 mg/tablet, among them the portion of the concentrations of sildenafil over 150 mg/tablet exceeded 88%. One case in tested samples contained demethylhongdenafil (90 mg/tablet). These results indicate that there were many fake anti-impotence drug contained high level of anti-impotence pharmaceutical ingredients, a sustainable monitoring and the blocked distribution of fake anti-impotence drugs recommended.

• Journal of Food Hygiene and Safety
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• v.32 no.2
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• pp.89-95
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• 2017

A rapid, sensitive analytical method for glucuronolactone in beverages was developed and validated using hydrophilic interaction liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HILIC-ESI-MS/MS). To determine the optimum analytical conditions for glucuronolactone, three different kinds of HILIC columns and two mobile phases with different pH values were examined. An amide-bonded stationary phase with a pH 9 acetonitrile-rich mobile phase was the best condition in terms of column retention, ESI-MS/MS response area, and signal-to-noise ratio. After extraction, glucuronolactone was separated through the HILIC amide column and detected by negative ESI-MS/MS in selected reaction monitoring (SRM) mode. Nine energy drinks sold in Korea were spiked with glucuronolactone at a concentration of 5 ng/mL; the Monster $Energy^{TM}$ sample showed the smallest peak area and its signal-to-noise ratio was used for method validation. Good linearity was obtained in the concentration range from 20 to 1500 ng/mL with a correlation coefficient > 0.998. The developed method had a limit of detection (LOD) of 6 ng/mL and a limit of quantitation (LOQ) of 20 ng/mL. The recovery of this method at concentration of 20, 100, 500, and 1000 ng/mL was 96.3%-99.2% with relative standard deviations (RSD) of 1.6%-14.0%. A reproducibility precision assessment at concentration of 100 and 500 ng/mL was carried out among three laboratories. The recovery of that evaluation was 95.1%-102.3% with RSD of 2.7%-7.0%. An analysis of variance indicated that there was no difference between the recovery results of the three laboratories at the 5% significance level. The validated method is applicable to inspecting beverages adulterated with glucuronolactone in Korea.

• Korean Journal of Environmental Agriculture
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• v.33 no.2
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• pp.111-120
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• 2014

BACKGROUND: This study was conducted to investigate the levels of pesticide residues in fruits and to assess their risk to human health. METHODS AND RESULTS: Monitoring of 215 samples of fruits collected from local markets in incheon during 2013 was performed. 259 pesticides were analyzed by multi-residue method and Quick, Easy, Cheap, Effective, Rugged, and safe/Mass/Mass(QuEChERS/MS/MS) method using Gas Chromatography-Electron Capture Detector/Nitrogen Phosphorus Detector(GC-ECD/NPD), GC-MS, LC(Liquid Chromatography-Mass/Mass(LC-MS/MS) and High Performance Liquid Chromatography-Photodiode Array/Fluorescence Detector(HPLC-PDA/FLD). In 56.3% of the samples detected pesticide residues and were not found to exceed Maximum Residue Limits(MRL). The highest detected samples were found in citrus fruits(83.9%). Among the detected compounds, carbendazim(13.1%), imazalil (11.7%), thiabendazole(10.7%) and fludioxonil(9.8%) were frequently found in fruits. A risk assessment of pesticide residues in fruits was performed by calculating Estimated Daily Intake(EDI) and Acceptable Daily Intake(ADI). Also, we were evaluated removal efficiency of pesticide residues by washing and peeling. The removal efficiency of pesticide residues in citrus and tropical fruits by peeling processes were 91.6%. After the washing process, the removal rates were 43.1%(Cherry, Grape, Blueberry). CONCLUSION: The level of pesticide residues in fruits was within the MRL. The range of %ADI values was from 0.00011 to 0.98795%. The process of washing or peeling reduces the level of pesticide residues. The results of this research concluded that the detected pesticides are not harmful to human being.

• Journal of Food Hygiene and Safety
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• v.37 no.4
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• pp.238-248
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• 2022

This study was conducted to evaluate the safety of 208 types of residue pesticides on 150 dried agricultural products in Ulsan. The pesticide residues were detected using GC-MS/MS, LC-MS/MS, GC/ECD, GC/NPD, and LC/PDA. The detection rate was 19.3% (29 of 150 samples), and 28 types of pesticides were detected. Two of the 29 pesticide residues exceeded the maximum residue limit (MRL). Difenoconazole was detected in Ulleungdo aster, and chlorothalonil and chlorpyrifos were detected in chili pepper leaves. In the vegetable group, the frequency of pesticide residues was found to be the highest in dried leafy vegetables, followed by dried fruiting vegetables other than cucurbit vegetables, and then dried stalk and stem vegetables. The pesticide types detected in the commercial dried agricultural products were fungicide (60%), insecticide (23.8%), and acaricide (16.3%). In the validation study, the values of limit of detection (LOD), limit of quantitation (LOQ), coefficient of determination (R²), and recovery rate were in the range of 0.0001-0.0409 mg/kg, 0.0003-0.1241 mg/kg, 0.994-0.999, and 81.58-116.79%, respectively. The ratio of estimated daily intake (EDI)/acceptable daily intake (ADI) was 0.00002-0.31395%.

• KSBB Journal
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• v.31 no.3
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• pp.165-170
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• 2016

This study was carried out for investigate that physiological activity, quantification and qualitative were sinigrin of Dolsan leaf mustard pickle (DLMP) during storage. sinigrin contains high amounts of nutritional and medicinal compounds, which are important for maintaining optimum health. ACE inhibitory activity was ranged between 43.2 and 79.4%. DLMP methanol extracts demonstrated highest ACE inhibitory activity at 79.4% on day 14, whereas DLMP ethanol extracts demonstrated highest Angiotensin I-converting Enzyme (ACE) inhibitory activity of 43.2% at day 0. The ${\alpha}-glucosidase$ inhibitory activity of positive control 0.02% (v/v) acarbose was 78%. The DLMP methanol extracts had the highest ${\alpha}-glucosidase$ inhibitory activity at 64.0% on day 14, whereas DLMP ethanol extracts had the lowest ${\alpha}-glucosidase$ inhibitory activity of 42.8% at day 28. Sinigrin was high in DLMP methanol extracts at $49.55{\mu}g/ml$ on day 14 of storage. Sinigrin standard was eluted at 2.73 min and MS analysis was m/z 283.03 along with fragment ions at m/z 204 and 149.06. These data show that sinigrin formed desulfo-glucosinolates $[M-SO_3-2H_2O+K+2H]^+$. Sinigrin concentration increased until day 14 and then decreased after that. DLMP methanol extracts had consistently higher sinigrin concentration than DLMP acetonitrile extracts during 28 days of storage.

• Journal of Food Hygiene and Safety
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• v.38 no.5
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• pp.390-401
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• 2023

Major components of lac coloring include laccaic acids A, B, C, and E. The Korean Food Additive Code regulates the use of lac coloring and prohibits its use in ten types of food products including natural food products. Since no commercial standards are available for laccaic acids A, B, C, and E, a standard for lac pigment itself was used to separate laccaic acids from the lac pigment molecule. A standard for each laccaic acid was then obtained by fractionation. To obtain pure lac pigment for use in food by High performance Liquid Chromatography Photo Diode Array (PDA), a C8 column yielded the best resolution among various tested columns and mobile phases. A qualitative analytical method using High Performance Liquid Chromatography (HPLC) Tandem Mass(LC-MS/MS) was developed. The conditions for fast and precise sample preparation begin with extraction using methanol and 0.3% ammonium phosphate, followed by concentration. The degree of precision observed for the analyses of ham, tomato juice and Red pepper paste was 0.3-13.1% (Relative Standard Deviation (RSD%)), degree of accuracy was 90.3-122.2% with r²=0.999 or above, and recovery rate was 91.6-114.9%. The limit of detection was 0.01-0.15 ㎍/mL, and the limits of quantitation ranged from 0.02 to 0.47 ㎍/mL. Lac pigment was not detected in 117 food products in the 10 food categories for which the use of lac pigment is banned. Multiple laccaic acids were detected in 105 food products in 6 food categories that are allowed to use lac color. Lac pigment concentrations range from 0.08 to 16.67 ㎍/mL.

• Korean Journal of Food Science and Technology
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• v.36 no.6
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• pp.872-878
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• 2004

Food products selected based on their annual sales and international acrylamide research data were analyzed for quantitation of acrylamide. Samples including raw food, substitute meal, snack, drink, and sauce products were analyzed by LC/MS/MS methods adopted by PDA. Upon comparison, concentrations of acrylamide in these products were similar to those analyzed in other countries.