• Journal of Food Hygiene and Safety
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• v.31 no.3
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• pp.186-193
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• 2016

An analytical method was developed for the determination of oxathiapiprolin in agricultural commodities. Oxathiapiprolin is a new oomycide (fungicide of piperidinyl thiazole isoxazoline class) which controls downy mildew in cucurbits caused by Pseudoperonospora cubensis (oomycete plant pathogen). Agricultural commodities were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, adjusting pH between 9 and 10 by 1 N sodium hydroxide. After purification by silica SPE cartridge to clean up the interference of organic compounds, they were finally quantified by HPLC-UVD (high performance liquid chromatograph ultraviolet detector) using a wavelength at 260 nm and confirmed by LC-MS (liquid chromatograph mass spectrometer) in electro-spray ionization positive ion mode. The standard calibration curve was linear with coefficients of determination ($r^2$) 1.00 over the calibration ranges (0.025-2.5 mg/L). Recoveries were ranged between 86.7 to 112.7%, with relative standard deviations less than 10% at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates. The overall results were determined and estimated according to the CODEX guidelines (CAC/GL40). The proposed method for determination of oxathiapiprolin residues in agricultural commodities can be used as an official method.

• Journal of Food Hygiene and Safety
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• v.24 no.1
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• pp.56-62
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• 2009

Patulin, a mycotoxin mainly produced by Penicillium and Aspergillus, is found in various foods. In the present, a maximum acceptable level for patulin is established at $50{\mu}g/kg(ppb)$ in apple juices and apple concentrates in Korea. But patulin may be detected in foods produced with other fruits. In the present study, patulin contamination was analyzed in 520 samples of fruit juices and beverages, and 50 samples of fruit juice concentrates. High performance liquid chromatography(HPLC) was applied to quantitatively analyze patulin levels in samples and liquid chromatography-mass spectrometry(LC/MS/MS) was used to remove false positive results. The results showed that three samples of 520 fruit juices and beverages and five samples of 50 fruit juice concentrates were contaminated by patulin, $9.8-18.0{\mu}g/kg$ and $4.7-18.2{\mu}g/kg$ respectively. Contaminated samples were produced with apple, orange or pear. This indicates that it is necessary to extend the regulatory range of patulin. In the other hands, the present study confirmed the effectiveness of LC/MS/MS analytical method to remove false positive results.

• Applied Biological Chemistry
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• v.15 no.2
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• pp.169-173
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• 1972

In five varietes of Citrus junos sieb grown in different area in Korea, the general components, total acids and inorganic components were calculated and compared with one other. In the orchard soils, the physical and chemical properties were studied. The results are summarized as follow: 1. Generally, the rind was weighter than tile flesh compared with the other fruits and the proportion of the rind was 49%. 2. Total contents of organic acids in rind and flesh were 12.29me and 39.79me respectively. 3. The order of the contents of inorganic components in the flesh and rind was $CaO>K_2O>MgO>P_2O_5>SO_4$ 4. The contents of crude protein and crude fat were increased with those of MgO and $SO_4$ in fruits. 5. The quantity of protein in the soil seed to influence greatly in rind formation not only in citrus fruits but also Citrus junos sieb. 6. In growing Citrus junos sieb, C.L. seemed to he the most adequate soil. 7. The pH range of the soil was from 5.05 to 7.20 generally. 8. The contents of crude protein and crude fat in citrus fruits seemed to be increased with those of organic material and total-nitrogen in the soil.

• 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.

• 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 Food Science and Technology
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• v.45 no.4
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• pp.391-402
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• 2013

Pesticide residues in agricultural products in Korea were evaluated to create a data base to inform food policy. Pesticide residues were investigated in 17 commodities collected from 9 provinces in 2012. Our analytical method of multiresidue analysis, involved the analysis of individual recovery, linearity, limit of detection, and limit of quantitation of 60 pesticides in six matrices. The pesticides, including acetamiprid and forchlorofenuron, were evaluated in 358 agricultural samples by liquid chromatography/tandem mass spectrometry. Twenty three pesticides were detected from 67 samples. The results showed that the ratio of estimated daily intake to acceptable daily intake was 0.00009-0.0861% by the intake assessment, which means that residual pesticides in agricultural products in Korea are properly controlled.

• Analytical Science and Technology
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• v.27 no.5
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• pp.234-242
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• 2014

Imicyafos which is a nematicide for controlling root-knot nematodes has been registered in the Republic of Korea in 2012, and the maximum residue limits of imicyafos are set to watermelon and korean melon as each 0.05 mg/kg. Extremely reliable and sensitive analytical method is required for ensuring food safety on imicyafos residues in agricultural commodities. Imicyafos residues in samples were extracted with acetone, partitioned with hexane and dichloromethane, and then purified with florisil. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. Linear range was between 0.1~5 mg/kg with the correlation coefficient ($r^2$) 0.99997. Average recoveries of imicyafos ranged from 77.0 to 115.4% at the spiked levels of 0.02 and 0.05 mg/kg with the relative standard deviations of 2.2~9.6%. Limit of detection and quantification were 0.005 and 0.02 mg/kg, respectively. An inter-laboratory study was conducted to validate the determination method in depth, and the results were satisfactory. All of the validation results revealed that the developed analytical method in this study is relevant for imicyafos determination in agricultural commodities and will be used as an official analytical method.

• Korean Journal of Environmental Agriculture
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• v.34 no.4
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• pp.318-327
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• 2015

BACKGROUND: Trinexapac-ethyl is a plant growth regulator (PGR) that inhibits the biosynthesis of plant growth hormone (gibberellin). It is used for the prevention of lodging, increasing yields of cereals, and reducing mowing of turf. The experiment was conducted to establish a determination method for trinexapac-ethyl and its metabolites trinexapac in agricultural products using LC-MS/MS.METHODS AND RESULTS: Trinexapac-ethyl and trinexapac were extracted from agricultural products with methanol/ distilled water and the extract was partitioned with dichloromethane and then detected by LC-MS/MS. Limit of detection(LOD) was 0.003 mg/kg and limit of quantification(LOQ) was 0.01 mg/kg, respectively. Matrix matched calibration curves were linear over the calibration ranges (0.01-1.0 mg/L) for all the analytes into blank extract withr²> 0.997. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, 10LOQ, 50LOQ,n=5). Recoveries of trinexapacethyl and trinexapac were within the range of 73.6-106.9%, 72.7-99.2%, respectively. The relative standard deviations (RSDs) were less than 9.0%. All values were consistent with the criteria ranges requested in the CODEX guideline(CAC/GL 40, 2003).CONCLUSION: The proposed analytical method was accurate, effective and sensitive for trinexapac-ethyl and trinexapac determination and it can be used to as an official method in Korea.

• Korean Journal of Environmental Agriculture
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• v.31 no.4
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• pp.300-307
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• 2012

BACKGROUND: The Transfer Factor (TF) of heavy metals from soil to plant is important, because TF is an indicator of heavy metal in soils and a factor that quantifies bioavailability of heavy metals to agricultural products. This study was conducted to investigate the transfer ability of Arsenic (As), Cadmium (Cd), and Lead (Pb) from soil to agricultural products. METHODS AND RESULTS: We investigated heavy metals (As, Cd and Pb) concentrations in 9 agricultural products (rice, barely, corn, pulse, lettuce, pumpkin, apple, pear, tangerin) and soil. TF of agricultural products was evaluated based on total and HCl-extractable soil concentration of As, Cd, and Pb. Regression analysis was used to predict the relationship of total and HCl-extractable concentration with agricultural product contents of As, Cd, and Pb. The result showed that TF was investigated average 0.006~0.309 (As), 0.002~6.185 (Cd), 0.003~0.602 (Pb). The mean TF value was the highest as rice 0.309 in As, lettuce 6.185, pear 0.717, rice 0.308 in Cd, lettuce 0.602, pumpkin 0.536 in Pb which were dependent on the vegetable species and cereal is showed higher than fruit-vegetables in As. CONCLUSION(S): Soil HCl-extractable concentration of As, Cd, and Pb had the larger effects on thier contents in agricultural products than total soil concentrations. We suggests that TF are served as influential factor on the prediction of uptake. Further study for uptake and accumulation mechanism of toxic metals by agricultural products will be required to assess the human health risk and need TF of more agricultural products.

• Food Science and Preservation
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• v.14 no.4
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• pp.414-418
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• 2007

The physicochemical characteristics and sensory properties of Deodeok wine, formed by leaching of Deodeok at room temperature for 180 days, were investigated over the following range of Deodeok levels: 10, 15 and 20% (all w/v). The higher the level of Deodeok, the greater were the final values of total sugars, reducing sugars, total polyphenols, and crude saponins. The Hunter's b-value (yellowness) of Deodeok wine varied markedly with Deodeok levels, and yellowness was highest in Deodeok wine containing 20% (w/v) Deodeok. Non-volatile compounds, that form the basis of the liquor tax law, were 0.64, 1.38 and 2.11% (all w/v), respectively, at day 160. Of these values, that of 2.11% (w/v), the level of non-volatile compounds in Deodeok wine containing 20% (w/v) Deodeok, was in accord with the liquor tax law (that requires this figure to be 2.0%). Sensory evaluation showed that Deodeok wine containing 20% (w/v) Deodeok was superior to the other wines tested.