• Korean Journal of Food Science and Technology
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• v.51 no.4
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• pp.301-308
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• 2019

The antioxidant properties of Eriobotrya japonica leaf extract were investigated using DPPH and ABTS radical scavenging assay. The 80% ethanol extract of leaves ($IC_{50}$ values for DPPH and ABTS were 13.9 and $10.9{\mu}g/mL$, respectively) and young leaves ($IC_{50}$ values for DPPH and ABTS were 20.7 and $17.3{\mu}g/mL$, respectively) showed high radical scavenging activity. Additionally, the quantitative method for estimation of ellagic acid and chlorogenic acid from E. japonica leaves was optimized by HPLC/DAD. This method showed high linearity of the calibration curve with a coefficient of correlation ($R^2$) equal to 0.999. The LOD values for ellagic acid and chlorogenic acid were 2.35 and $0.73{\mu}g/mL$, respectively, whereas LOQ values were 7.13 and $2.22{\mu}g/mL$, respectively. Recovery of the two compounds was 99.7-108.0% with RSD values less than 5.31%. These results suggest that 80% ethanol extract of E. japonica leaves could serve as a potential source of natural antioxidant for us in various industrial applications.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.263-268
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• 2019

Methanol is a toxic alcohol used in various products such as antifreeze, detergent, disinfectant and industrial solvent. In the human body, methanol is oxidized to formaldehyde and formic acid, which can lead to metabolic acidosis, optic nerve impairment, and death. In this study, the methanol levels in detergents (n=191) and rinse aids (n=13) were analyzed by gas chromatography-headspace-mass spectrometry (GC-HS-MS). Limit of detection was 1.09 mg/kg, accuracy and precision were 91.1-97.9% and <10%, and it was suitable for quantitative analysis. This analysis method was simple and fast with a higher recovery rate than the conventional MFDS (Ministry of Food and Drug Safety) method of diluting the sample in water and putting it in a headspace vial.

• Korean Journal of Environmental Agriculture
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• v.42 no.3
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• pp.203-210
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• 2023

Ferimzone Z is a fungicide for effectively controlling rice blast. Under light irradiation conditions, it undergoes a rapid conversion to its E-stereoisomer. Given the importance of isomers in risk assessments of residues in crops, an analytical method was developed for individual isomer quantification. A comparative analysis performed using two columns in HPLC-MS/MS demonstrated that the isomers were successfully separated using the Cadenza column. For the brown rice sample preparation, 5 g of the homogenized sample was saturated with 7 mL of water. The sample was then extracted with a 10 mL mixed solvent of acetonitrile and ethyl acetate (1:1, v/v) that contained 0.1% formic acid, and it was subsequently partitioned with magnesium sulfate and sodium chloride. The upper layer was purified using dSPE containing C₁₈ and PSA sorbents. The established method was subjected to method validation, and it showed recovery rates of 90.6-98.8% (RSD ≤ 3.9%) at concentrations of 0.01, 0.1, 2 mg/kg, with a soft matrix effect (%ME) ranging from -3.1% to +6.5%. This method can be employed in monitoring studies of brown rice to determine the conversion ratio from the Z isomers to the E isomers.

• Journal of Food Hygiene and Safety
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• v.38 no.3
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• pp.89-98
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• 2023

Currently, no guidelines exist regarding the maximum residues of pesticides in edible oil which is a processed food commonly consumed in Korea. This lack of guidelines hinders the evaluation of the safety of edible oil in terms of pesticide contamination. In this study, an analysis method based on heat distillation and GC-MS/MS was established by optimizing the extraction and purification procedure for 68 pesticides. Important variables in the thermal distillation procedure included heating temperature and time, and we found the nitrogen flow rate as a mobile phase and the type of dissolving solvent were not considerably affected. The determination coefficient (R²) of the residual pesticide was 0.99 or higher, and the quantitative limit (LOQ) was 0.01-0.02 mg/L. The average recovery rate (n=5) was 66.1-120.0% and the relative standard deviation was lower than ±10% when 68 pesticides were spiked at concentrations of 0.01-0.02, 0.1, and 0.5 mg/L. In addition, the within-laboratory precision was less than ±11%, meeting the Korea Food and Drug Safety Evaluation Institute's Guidelines on Standard Procedures for Preparing Food Testing Methods (2016). Therefore, the test method developed in this study can be used as a test method for managing the safety of the residual pesticide concentration in edible oil.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.10 no.3
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• pp.151-162
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• 1977

Distribution of marine algae is diverse in Korea and the resource of edible algae is abundant marking 239,037 tons of yearly production in 1976. They have been known as a protein source and used as a supplement in Korean diet. It is necessary to estimate the potentiality and properties of usable algal proteins especially as food resources and studies of extraction and separation of the proteins, therefore, are basically required for this purpose. In this study, the influence of various factors including the sample treatment, extraction time and temperature, sample us extraction solvent ratio and pH upon the extractability of the water soluble protein was determined. And the effect of precipitation treatment for isolation of the algal protein from the extracts was also tested. Nine species of algae, the major ones in consumption as food namely Porphyra suborbiculata, Undaria pinnatifida, Hizikia fusiforme, Sargassum fulvellu, Enteromorpha linza, Codium fragile, Sargassum kjellmanianum and Ulva pertusa were collected as fresh from Kijang, Yangsan Gun, in the vicinity of Busan city. The content of crude protein $(N\times6.25)$ of the algae ranged from $9.46\%\;to\;24.14\% showing the highest value in Porphyra suborbiculata and the minimum in Hizikia fusiforme. In the effort of maceration of blending methods on the extractability, immersion freezing in dry ice-methanol solution appeared most effective yielding 1.5 to 2.5 times extractability than that of the mortar grinding method. The effect of the ratio of sample vs solvent on extractability differed from species. It was enhanced at the ratio of 1:20 (w/v) in Ulva pertusa and Enteromorpha linza while the ratio was 1:30 (w/v) for Cedium fragile, Undaria pinnatifida, Hizikia fusiferme, Sargassum fulvellum and Porphyra suborbiculata and 1:40 for Sargassum kjellmanianum respectively. The effect of extraction time and temperature was revealed differently from species which might be caused by differences in the constitution of algal tissues resulting in that the extraction for 1 hour at $50^{\circ}C$ gave the maximum extractabilily in Ulva pertusa and Enteromorpha linza, 2 hours in Porphyra suborbiculata, Hikikia fusiforme, Undaria pinnatifida, Sargassum kjellmanianum and 3 hours in Codium fragile. And the extractability was higher at $50^{\circ}C$ to $60^{\circ}C$ for the most of the tested samples except Hizikia fusiforme. The optimum pH for the extraction was 9 to 12. The recovery of extractable nitrogen to the total nitrogen was $63\%$ in average with the first extracts and $8.6\%$ with the second extracts respectively. Both extracts were prepared by 2 hour extraction at $50{\pm}1^{\circ}C$ with dry ice-methanol frozen and seasand macerated materials. And these conditions assumed to be an optimum for the extraction of water soluble algal proteins since the nitrogen content after the first extraction covered $90\%$ of the total water extractable nitrogen. In the precipitation of the extracted proteins, Barnstein method and methanol treatment seemed to be more efficient than other precipitation methods.

• Analytical Science and Technology
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• v.36 no.6
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• pp.291-299
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• 2023

The benzo[a]pyrene in edible oils is extracted using methods such as Liquid-liquid, soxhlet and ultrasound-assisted extraction. However these extraction methods have significant drawbacks, such as long extraction time and large amount of solvent usage. To overcome these drawbacks, this study attempted to improve the current complex benzo[a]pyrene analysis method by applying the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method that can be analyzed in a simple and short time. The QuEChERS method applied in this study includes extraction of benzo[a]pyrene into n-hexane saturated acetonitrile and n-hexane. After extraction and distribution using magnesium sulfate and sodium chloride, benzo[a]pyrene is analyzed by liquid chromatography with fluorescence detector (LC/FLR). As a result of method validation of the new method, the limit of detection (LOD) and quantification (LOQ) were 0.02 ㎍/kg and 0.05 ㎍/kg, respectively. The calibration curves were constructed using five levels (0.1~10 ㎍/kg) and coefficient (R²) was above 0.99. Mean recovery ratio was ranged from 74.5 to 79.3 % with a relative standard deviation (RSD) between 0.52 to 1.58 %. The accuracy and precision were 72.6~79.4 % and 0.14~7.20 %, respectively. All results satisfied the criteria ranges requested in the Food Safety Evaluation Department guidelines (2016) and AOAC official method of analysis (2023). Therefore, the analysis method presented in this study was a relatively simple pretreatment method compared to the existing analysis method, which reduced the analysis time and solvent use to 92 % and 96 %, respectively.

• Journal of Food Hygiene and Safety
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• v.36 no.3
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• pp.220-227
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• 2021

Fluoroimide is a fungicide and is also used as a pesticide for persimmons and potatoes. The established fluoroimide pesticide analysis method takes a long time to perform and uses benzene, a carcinogen. In addition, a lower limit of quantification is required due to enforcement of the Positive List System. Therefore, this study aimed to improve the analysis method for residual fluoroimide to resolve the problems associated with the current method. The analytical method was improved with reference to the increased stability of fluoroimide under acidic conditions. Fluoroimide was extracted under acidic conditions by hydrogen chloride (4 N) and acetic acid. MgSO₄ and NaCl were used with acetonitrile. C₁₈ (octadecylsilane) 500 mg and graphitized carbon black 40 mg were used in the purification process. The experiment was conducted with agricultural products (hulled rice, potato, soybean, mandarin, green pepper), and liquid chromatograph-tandem mass spectrometry was used for the instrumental analysis. Recovery of fluoroimide was 85.7-106.9% with relative standard deviations (RSDs) of less than 15.6%. This study reports an improved method for the analysis of fluoroimide that might contribute to safety by substituting the use of benzene, a harmful solvent. Furthermore, the use of QuEChERS increased the efficiency of the improved method. Finally, this research confirmed the precise limit of quantification and these results could be used to improve the analysis of other residual pesticides in agricultural products.

• Resources Recycling
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• v.31 no.1
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• pp.65-77
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• 2022

A study was conducted in Korea on the leaching behavior and possibility of recovery of vanadium and other valuable metals from domestic vanadium titanomagnetite (VTM) by direct acid leaching. In this study, a VTM concentrate containing 0.8% V₂O₅ was used, and the ratio of magnetite to ilmenite was calculated as 1.9:1 by using the HSC program. The leaching behavior of vanadium from the VTM was similar to that of iron, and it was affected by the concentration of sulfuric acid and temperature. Further, titanium could be leached in the form of TiOSO₄ at a temperature higher than 75℃. To improve the leaching efficiency of V, Fe, and Ti in VTM, reductive sulfuric acid and oxidative sulfuric acid leaching were performed. When Na₂SO₃ was used as a reducing agent, the leaching rate of vanadium was 80% of that in that case of leaching by sulfuric acid. Similarly, the leaching rate of titanium increased from 20% to 50%. When Na₂S₂O₈ was used as an oxidation agent, most of the vanadium was leached, and the main residue found by XRD analysis was ilmenite. In studies on the possibility of recovering valuable metals, the selective extraction of metals is hardly achieved by solvent extraction from oxidation leaching solutions; however, in this study, Cyanex 923, a solvation extractant from reductive leaching solutions, could selectively extract Ti.

• Journal of Food Hygiene and Safety
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• v.37 no.6
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• pp.373-384
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• 2022

Fluoxastrobin a fungicide developed from Strobilurus species mushroom extracts, can be used as an effective pesticide to control fungal diseases. In this study, we optimized the extraction and purification of fluoxastrobin according to its physical and chemical properties using the QuEChERS method and developed an LC-MS/MS-based analysis method. For extraction, we used acetonitrile as the extraction solvent, along with MgSO₄ and PSA. The limit of quantitation of fluoxastrobin was 0.01 mg/kg. We used 0.01, 0.1, and 0.5 mg/kg of five representative agricultural products and treated them with fluoxastrobin. The coefficients of determination (R²) of fluoxastrobin and fluoxastrobin Z isomer were > 0.998. The average recovery rates of fluoxastrobin (n=5) and fluoxastrobin Z isomer were 75.5-100.3% and 75.0-103.9%, respectively. The relative standard deviations (RSDs) were < 5.5% and < 4.3% for fluoxastrobin and fluoxastrobin Z isomer, respectively. We also performed an interlaboratory validation at Gwangju Regional Food and Drug Administration and compared the recovery rates and RSDs obtained for fluoxastrobin and fluoxastrobin Z isomer at the external lab with our results to validate our analysis method. In the external lab, the average recovery rates and RSDs of fluoxastrobin and fluoxastrobin Z isomer at each concentration were 79.5-100.5% and 78.8-104.7% and < 18.1% and < 10.2%, respectively. In all treatment groups, the concentrations were less than those described by the 'Codex Alimentarius Commission' and the 'Standard procedure for preparing test methods for food, etc.'. Therefore, fluoxastrobin is safe for use as a pesticide.

• Journal of Sericultural and Entomological Science
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• no.11
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• pp.23-29
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• 1970

This experiment is to improve the wrinkle recovery (W.R.) of silk fabrics. The silk fabrics is creased very well, and the crease is the serious defection of it. This experiment is to improve the nature by use of formaldehyde on fabrics. The reagents used were HCl, CH$_3$COOH, CaC$_2$, HCHO, Na$_2$CO$_3$, NH$_4$OH, NaOH and NaHCO$_3$. The silk fabrics was treated, to compare 1 he influence of conditions, by varying the quantities of reagents and the temperature of solution, and the reaction time. The cotton fabrics and the viscose rayon were sunk with the silk at the same condition to be compared the influence. 1) Those of the most suitable temperature to improve for the better W.R. are 75$^{\circ}C$ for silk, 35-45$^{\circ}C$ for cotton, and no particular temperature under 75$^{\circ}C$ for viscose rayon. 2) The W.R. improvements after treated at the temperature of 1) were 11％ for silk and 33.4％ for cotton. 3) There are the best treating time for every fabrics. They were 60 to 90 min. for viscose rayon when HAC Ras used for solvent. It took, however, 60min. of the best time for silk, 120 min. for cotton, and 40 min. for viscose rayon when acetic anhydride instead of HAC was used. 4) It was possible to improve 16.6％ of W.R. for silk at the most suitable treating time, 25.0％ for cotton, and 13.3％ for viscose rayon. 5) Acetic anhydride was rather more effective to improve W.R. of both silk and viscose rayon than HAC. 6) Treating time was also shorter in case of using acetic anhydride than HAC. 7) The improvement of W.R. were 8.3％ for silk at the 10 to 14 ml. of HCHO the best volume, 21. 5％ for cotton at 18m!. of HCHO, and 70％ of for viscose rayon at 14 to 18ml. of HCHO. 8) The most effective quantity of HCI is 14 ml. for both silk and cotton. The W.R. improvement of silk was 22.2％, and that of cotton 19.5％. 9) The W.R. of 83.3％ the best for silk and 61. 6％ for cotton were gained when 4.2gr. of NaHCO$_3$ brings down the percent of W.R. for both silk and cotton. 10) The more NaOH and NH$_4$OH as neutralizing agents, the less effectivity of W.R. until the quantities of the reagents are reached to a special range which are 3. 3m!. for silk and 3.3-6.6 ml. for cotton, and then we can see the W.R. increasing as the quantities of reagents are increased. These facts were evident in case of silk and cotton. We can also see with this fact that the reminder of 〔OH$\^$-/〕 neutralizing 〔CH$\^$+/〕in solution makes it possible to treat formaldehyde on fabrics. 11) Low curing temperature was comparatively better for silk, and high temperature better for cotton. 12) The result of this experiment shows that the Improvement of W.R. for silk was possible to 94％ which means 22％ W.R. increase compared to the untreated silk. This effect also shows that the improvement to W '||'&'||' W (wash and wear) of silk will be possible.