• Journal of the Korean Society of Food Science and Nutrition
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• v.46 no.3
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• pp.358-367
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• 2017

Preservatives, as food additives, are occasionally intrinsic to natural raw materials or sometimes generated during the fermentation process as reported in many research articles. Preservative compounds in raw food materials may persist in the final food product, which is not supposed to include such preservative compounds. In this study, we validated an analytical method for preservative compounds in raw materials of functional foods. Quantification of benzoic acid and sorbic acid was determined using HPLC-PDA analysis after distillation, whereas propionic acid was quantified with GC-FID. A significant set of validation data (accuracy, precision, linearity, recovery, etc) was acquired. A total of 212 samples were collected for analysis of naturally occurred preservatives, and preservatives were detected in 85 samples. Most of the detected samples showed less 10 mg/kg of preservatives. The results of this study provide fundamental data on naturally occurring preservatives in raw materials of functional foods. Moreover, building up a database of naturally occurring preservatives could solve problems in the current scientific data.

• Journal of the Korean Society for Marine Environment & Energy
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• v.15 no.3
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• pp.208-218
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• 2012

Numerical simulation technique has been developed to calculate microwave backscattering from water surface. The simulation plays a role of a substitute for experiments. Validation of the simulation was shown by comparing with experimental results. Water area observations by microwave radar have been simulated to evaluate algorithms and systems. Furthermore, the simulation can be used to understand microwave scattering mechanism on the water surface. The simulation has applied to the various methods for water area observations, and the utilizations of the simulation are introduced in this paper. In the case of fixed radar, we show following examples, 1. Radar image with a pulse Doppler radar, 2. Effect of microwave irradiation width and 3. River observation (Water level observation). In addition, another application (4.Synthetic aperture radar image) is also described. The details of the applications are as follows. 1. Radar image with a pulse Doppler radar: A new system for the sea surface observation is suggested by the simulation. A pulse Doppler radar is assumed to obtain radar images that display amplitude and frequency modulation of backscattered microwaves. The simulation results show that the radar images of the frequency modulation is useful to measure sea surface waves. 2. Effect of microwave irradiation width: It is reported (Rheem[2008]) that microwave irradiation width on the sea surface affects Doppler spectra measured by a CW (Continuous wave) Doppler radar. Therefore the relation between the microwave irradiation width and the Doppler spectra is evaluated numerically. We have shown the suitable condition for wave height estimation by a Doppler radar. 3. River observation (Water level observation): We have also evaluated algorithms to estimate water current and water level of river. The same algorithms to estimate sea surface current and sea surface level are applied to the river observation. The simulation is conducted to confirm the accuracy of the river observation by using a pulse Doppler radar. 4. Synthetic aperture radar (SAR) image: SAR images are helpful to observe the global sea surface. However, imaging mechanisms are complicated and validation of analytical algorithms by SAR images is quite difficult. In order to deal with the problems, SAR images in oceanic scenes are simulated.

• Journal of the Korean Society of Food Science and Nutrition
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• v.45 no.1
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• pp.61-67
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• 2016

An HPLC analysis method was developed for standard determinations of chlorogenic acid, 3,4-di-O-caffeoylquinic acid, 3,5-di-O-caffeoylquinic acid, and 4,5-di-O-caffeoylquinic acid as functional health materials in Ligularia fischeri extract. HPLC was performed on a $C_{18}$ Kromasil column ($4.6{\times}250mm$, $5{\mu}m$ column) with a gradient elution of 0.1% (v/v) trifluoroacetic acid and acetonitrile at a flow rate of 1.0 mL/min at $30^{\circ}C$. The analytes were detected at 330 nm. The HPLC method was validated in accordance with the International Conference on Harmonization guideline of analytical procedures with respect to specificity, precision, accuracy, and linearity. The limits of detection and quantitation for the four compounds were 3.0~14.6 and $9.2{\sim}44.4{\mu}g/mL$, respectively. Calibration curves showed good linearity ($r^2$ > 0.999), and the precision of analysis was satisfied (less than 0.9%). Recoveries of quantified compounds ranged from 98.96 to 101.81%. This result indicates that the established HPLC method is very useful for the determination of marker compounds in Ligularia fischeri leaf extracts.

• Journal of the Korean Society of Food Science and Nutrition
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• v.46 no.2
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• pp.210-219
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• 2017

This study aimed to establish an optimal extraction process and high-performance liquid chromatography (HPLC)-photodiode array (PDA) analytical method for determination of marker compounds, dihydrokaempferol (DHK) and 3-O-methylquercetin (3-MeQ), as a part of materials standardization for the development of health functional foods from stems of Opuntia ficus-indica var. saboten (OFS). The quantitative determination method of marker compounds was optimized by HPLC analysis, and the correlation coefficient for the calibration curve showed very good linearity. The HPLC-PDA method was applied successfully to quantification of marker compounds in OFS after validation of the method in terms of linearity, accuracy, and precision. Ethanolic extracts from stems of O. ficus-indica var. saboten (OFSEs) were evaluated by reflux extraction at 70 and $80^{\circ}C$ with 50, 70, and 80% ethanol for 3, 4, 5, and 6 h. Among OFSEs, OFS70E at $80^{\circ}C$ showed the highest contents of DHK and 3-MeQ of $26.42{\pm}0.65$ and $3.88{\pm}0.29mg/OFS100g$, respectively. Furthermore, OFSEs were determined for their antioxidant activities by measuring 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging and lipid peroxidation (LPO) inhibitory activities in rat liver homogenate. OFS70E at $70^{\circ}C$ showed the most potent antioxidant activities with $IC_{50}$ values of $1.19{\pm}0.11$ and $0.89{\pm}0.09mg/mL$ in the DPPH radical scavenging and LPO inhibitory assays, respectively. To identify active components of OFS, various chromatographic separation of OFS70E led to isolation of 11 flavonoids: dihydrokaempferol, dihydroquercetin, 3-O-methylquercetin, quercetin, isorhamnetin 3-O-glucoside, isorhamnetin 3-O-galactoside, narcissin, kaempferol 7-O-glucoside, quercetin 3-O-galactoside, isorhamnetin, and kaempferol 3-O-rutinoside. The results suggest that standardization of DHK in OFSEs using HPLC-PDA analysis would be an acceptable method for the development of health functional foods.

• Journal of the Korean Society of Food Science and Nutrition
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• v.45 no.11
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• pp.1610-1616
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• 2016

This study aimed to establish an optimal extraction process and high performance liquid chromatography-ultraviolet (HPLC-UV) analytical method for determination of 3,5-dicaffeoylquinic acid (3,5-DCQA) as a part of materials standardization for the development of a xanthine oxidase inhibitor as a health functional food. The quantitative determination method of 3,5-DCQA as a marker compound was optimized by HPLC analysis using a Luna RP-18 column, and the correlation coefficient for the calibration curve showed good linearity of more than 0.9999 using a gradient eluent of water (1% acetic acid) and methanol as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 320 nm. The HPLC-UV method was applied successfully to quantification of the marker compound (3,5-DCQA) in Aster glehni extracts after validation of the method with linearity, accuracy, and precision. Ethanolic extracts of A. glehni (AGEs) were evaluated by reflux extraction at 70 and $80^{\circ}C$ with 30, 50, 70, and 80% ethanol for 3, 4, 5, and 6 h, respectively. Among AGEs, 70% AGE at $70^{\circ}C$ showed the highest content of 3,5-DCQA of $52.59{\pm}3.45mg/100g$ A. glehni. Furthermore, AGEs were analyzed for their inhibitory activities on uric acid production by the xanthine/xanthine oxidase system. The 70% AGE at $70^{\circ}C$ showed the most potent inhibitory activity with $IC_{50}$ values of $77.01{\pm}3.13{\sim}89.96{\pm}3.08{\mu}g/mL$. The results suggest that standardization of 3,5-DCQA in AGEs using HPLC-UV analysis would be an acceptable method for the development of health functional foods.

• Korean Journal of Environmental Agriculture
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• v.33 no.4
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• pp.388-394
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• 2014

BACKGROUND: Aclonifen is used as a systemic and selective herbicide to control a wide spectrum broad-leaf weeds by inhibition carotenoid biosynthesis, and then its MRLs(Maximum Residue Limits) will be determined in onion and garlic. In this study, a new official method was developed for aclonifen determination in agricultural products to routinely inspect the violation of MRL as well as to evaluate the terminal residue level. METHODS AND RESULTS: Aclonifen was extracted from crop samples with acetone and the extract was partitioned with dichloromethane and then purified by silica solid phase extraction(SPE) cartridge. The purified samples were detected GC using an ECD detector. Limits of detection(LOD) was 0.001 mg/kg and quantification(LOQ) was 0.005 mg/kg, respectively. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n=5). The recoveries were ranged from 74.3 to 95.0% with relative standard deviations(RSDs) of less than 8%. All values were consistent with the criteria ranges requested in the Codex guidelines(CAC/GL 40). CONCLUSION: The proposed analytical method was accurate, effective and sensitive for aclonifen determination and it will be used to as an official method in Korea.

• Korean Journal of Food Science and Technology
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• v.45 no.3
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• pp.285-292
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• 2013

This study was carried out to validate the safety of ametoctradin residues in agricultural commodities by developing an official analysis method. An analytical method was developed and validated using HPLC-PDA detectors. The samples were extracted with methanol, subsequently partitioned with dichloromethane and purified with florisil column chromatograph using acetone/hexane (30/70, v/v) as solvent. The method was validated by using grape, hulled rice, mandarin, and potato spiked with ametoctradin at 0.05 and 5.0 mg/kg, and pepper at 0.05 and 2.0 mg/kg. Average recoveries were 76-114.8% with relative standard deviation less than 10%, and the limit of detection and limit of quantification were 0.0125 and 0.05 mg/kg, respectively. The result of recoveries and overall coefficient of variation of the laboratory results from Gwangju regional Food and Drug Administration (FDA) and Daejeon regional FDA was accorded with Codex Alimentarius Commission Guideline (CAC/GL 40). Based on these results, this method was found to be appropriate for ametoctradin residue determination and can be used as the official method of analysis.

• Journal of Food Hygiene and Safety
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• v.30 no.2
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• pp.143-149
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• 2015

This study was conducted to simultaneous analysis methods for water soluble vitamins B group (vitamin $B_1$, vitamin $B_2$, nicotinic acid, nicotinamide, vitamin $B_6$) which is used as health functional foods etc. Analytical methods of water-soluble vitamins B group by HPLC were established through instrumental analytical conditions, and the examination of data such as domestic and foreign reliable methods, and papers of journal. HPLC method analyzing water soluble vitamins B group was established using Capcell Pak C18 UG 120 column in 270 nm through test of columns. The validation has been performed on the method to determine linearity, accuracy, limits of quantification (LOQ) and repeatability for water soluble vitamins B group. An excellent linearity ($r^2=0.999$) was observed for vitamin $B_1$, vitamin $B_2$, nicotinic acid, nicotinamide, vitamin $B_6$ in the concentration range ($0.1{\sim}2{\mu}g/mL$). Observed recovery of vitamin $B_1$ was found to be between 100 and 103%, vitamin $B^2$ was found to be between 104 and 112%, nicotinic acid was found to be between 82 and 85%, nicotinamide was found to be between 121 and 124% and vitamin $B_6$ was found to be between 95 and 104%. LOQ of vitamin $B_1$ was found to be $0.04{\mu}g/mL$, vitamin $B_2$ was found to be $0.05{\mu}g/mL$, nicotinic acid was found to be $0.15{\mu}g/mL$, nicotinamide was found to be $0.08{\mu}g/mL$ and vitamin $B_6$ was found to be $0.63{\mu}g/mL$. Repeatability precision for vitamin $B_1$ was found to be 0.4%, vitamin $B_2$ was found to be 0.4%, nicotinic acid was found to be 0.5%, nicotinamide was found to be 0.7% and vitamin $B_6$ was found to be 0.4% relative standard deviation (RSD). Also, verify the accuracy of the simultaneous analysis methods, we monitored the labeled contents of the health functional foods and children's preferred foods.

• 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.

• Food Science and Preservation
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• v.24 no.8
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• pp.1103-1112
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• 2017

This study was performed to investigate the effects of different cooking methods (boiling, roasting, stir-frying, and deep-frying) on folate retention in 6 kinds of mushrooms (Beech-, button-, Juda's ear-, oak-, oyster-, and winter-mushrooms) frequently consumed in Korea. In order to assure reliability of analytical data, trienzyme extraction-L casei method was verified and analytical quality control was also evaluated. Folate contents of mushrooms varied by 6.04-64.82 g/100 g depending on the type of mushrooms. and were significantly affected by cooking methods. Depending on cooking methods, folate contents of mushrooms decreased by 22-48%, 2-31%, and 17-56% for Juda's ear-, oak- and oyster-mushrooms, respectively, while 17-90% of folate was increased in Beech mushroom. Overall, the largest weight loss was found in boiled mushrooms, but the lowest one in deep-fried samples. True folate retention rates considering processing factor were less than 100% for all cooked mushrooms except for Beech samples. Overall, folate loss was the largest by boiling with water but the smallest by deep-frying. Both accuracy and precision of trienzyme extraction-L-casei method were excellent based on a recovery close to 100% and coefficient variations less than 3%. Quality control chart of folate analysis (n=26) obtained during the entire study and an international proficiency test (z-score=-0.5) showed that trienzyme extraction-L casei method is reliable enough for production of national folate database.