• 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.

• Journal of the Korean Society of Food Science and Nutrition
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• v.44 no.1
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• pp.85-88
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• 2015

This study attempted to establish an HPLC analysis method for determination of marker compounds as a part of material standardization for the development of health functional food materials from Perilla frutescens Britton var. acuta Kudo. The quantitative determination method of rosmarinic acid as a marker compound of P. frutescens Britton var. acuta Kudo extract (PFE) was optimized by HPLC analysis using a C18 column ($4.6{\times}150mm$, $5{\mu}m$) with 0.1% acetic acid as the elution gradient and methanol as the mobile phase at a flow rate of 1 mL/min and detection wavelength of 280 nm. The HPLC/UV method was applied successfully to quantification of the marker compound in PFE after validation of the method with linearity, accuracy, and precision. The method showed high linearity in the calibration curve at a coefficient of correlation ($R^2$) of 0.9995, and the limit of detection and limit of quantitation were $0.36{\mu}g/mL$ and $1.2{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 3.21% and 1.43%, respectively. Recovery rate test at rosmarinic acid concentrations of 12.5, 25 and $50{\mu}g/mL$ scored between 97.04~98.98% with RSD values from 0.25~1.97%. These results indicate that the established HPLC method is very useful for the determination of marker compound in PFE to develop a health functional material.

• Journal of Food Hygiene and Safety
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• v.33 no.6
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• pp.466-473
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• 2018

An analytical method of sodium polyacrylate in processed food products was developed and monitored by using size-exclusion chromatography. GF-7M HQ column and UV/VIS detector were selected based on peak shape and linearity. Flow rate, column oven temperature, and mobile phase were selected as 0.6 mL/min, $45^{\circ}C$, and 50 mM sodium phosphate buffer of pH 9.0, respectively. Samples for analysis of sodium polyacrylate were extracted with 50 mM sodium phosphate buffer of pH 7.0 for 3 hr at $20^{\circ}C$ and 150 rpm. Analytical method validation revealed proper selectivity and calibration curve was selected in the range of 50-500 mg/L, and correlation coefficient of calibration curve was more than 0.9985. Limit of detection of sodium polyacrylate was 10.95 mg/kg and limit of quantification was 33.19 mg/kg. Accuracy and coefficient of variation for sodium polyacrylate analysis was 99.6-127.6%, 3.0-8.3% for intra-day and 94.3-121.9%, 1.3-2.6% for inter-day, respectively. Sodium polyacrylate was detected in 40 samples among monitored 125 processed food products. Detected contents were less than 0.2%, limited by the Food Additives Code. Results suggest the established size-exclusion chromatography method could be used to analyze sodium polyacrylate in processed food products.

• Journal of Food Hygiene and Safety
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• v.37 no.4
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• pp.216-224
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• 2022

This study was aimed at validating the analysis methods for deacetylasperulosidic acid (DAA), total sugar, galacturonic acid, glucose, and galactose, which are the indicator components of fermented Morinda citrifolia polysaccharide extract (Vitalbos). We modified the previously reported methods for validating the analytical methods. The specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) were measured using phenol-sulfuric acid method and high-performance liquid chromatography (HPLC). The retention time and spectrum of the standard solution of Vitalbos coincided, confirming the specificity. The calibration curve correlation coefficient (R²), of five indicator components, ranged from 0.9995-0.9998, indicating excellent linearity of 0.99 or more. The intra-day and inter-day precision range of the assay was 0.14-3.01%, indicating a precision of less than 5%. The recovery rate was in the range of 95.13-105.59%, presenting excellent accuracy. The LOD ranged from 0.39 to 0.84 ㎍/mL and the LOQ ranged from 1.18 to 2.55 ㎍/mL. Therefore, the analytical method was validated for DAA, total sugar, galacturonic acid, glucose, and galactose, in Vitalbos. The indicator component content in Vitalbos was determined using a validated method. The contents of DAA, total sugar, galacturonic acid, glucose, and galactose were 2.31±0.06, 475.92±5.95, 72.83±1.05, 71.63±2.44, and 67.30±2.31 mg/g of dry weight, respectively. These results suggest that the developed analytical method is efficient and could contribute to the quality control of Vitalbos, as a healthy functional food material.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.210-217
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• 2015

Ipfencarbazone is a herbicide of the tetrazolinone class, and is believed to be an inhibitor of very long chain fatty acids (VLCFAs), which control cell division in weeds. The objective of this study was to develop and validate an official analytical method for ipfencarbazone determination in agricultural products. The ipfencarbazone residues in agricultural products were extracted with acetone, partitioned with n-hexane, and then purified through silica SPE cartridge. Finally, the analyte was quantified by gas chromatograph-electron capture detector (GC-ECD) and confirmed with gas chromatograph/mass spectrometer(GC/MS). The linear range of ipfencarbazone was 0.01 to 1.0 mg/L with the coefficient of determination ($r^2$) of 0.9999. The limit of detection (LOD) and quantification (LOQ) was 0.003 and 0.01 mg/kg, respectively. In addition, average recoveries of ipfencarbazone ranged from 80.6% to 112.3% at the different concentration levels LOQ, 10LOQ and 50LOQ, while the relative standard deviation was 2.2-8.6%. All values were consistent with the criteria ranges requested in the CODEX guidelines. Furthermore, and inter-laboratory study was conducted to validate the method. This proposed method for determination of ipfencarbazone residues in agricultural products can be used as an official analytical method.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.161-173
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• 2015

The multiresidue method 4.1.2.2 in Korea Food Code was extended for the analysis of 24 unregistered pesticide residues. The method includes acetonitrile extraction, liquid-liquid partition, Florisil SPE clean-up and GC analysis. The limits of quantification (LOQ) range of the method was 0.02~0.05 mg/kg for orange, brown rice and banana. The linearity for targeted pesticides were $R^2$ > 0.99 at the level ranged from 0.05 to 5 mg/L. Recovery test was performed at two concentration levels of LOQ and 4~10 times of LOQ. Recoveries and relative standard deviations (RSDs) of target pesticides were acceptable, showing 70~120% range and less than 20%, respectively, except for ethiprole, picloram and sulcotrion. This method is effectively applicable to routine analysis of target pesticides in orange, brown rice and banana.

• The Korean Journal of Pesticide Science
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• v.17 no.4
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• pp.314-334
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• 2013

This study explored an efficient modified Quick, Easy, Cheap, Effective, Rugged and safe (QuEChERS) method combined with liquid chromatography-electrospray ionization with tandem mass spectrometric detection for the analysis of residues of 76 pesticides in brown rice, barley and corn including acidic sulfonylurea herbicides. Formic acid (1%) acid in acetonitrile and dispersive solid phase extractions used for extraction of pesticides and clean-up of the extract respectively. Two fortified spikes at 50 and 200 ng $g^{-1}$ levels were performed for recovery test. Mean recoveries of majority of pesticides at two spike levels ranged from 73.2 to 132.2, 80.9 to 136.8, 66.6 to 143.5 for brown rice, barley and corn respectively with standard error (CV) less than 10%. Good linearity of calibration curves were achieved with $R^2$ > 0.9907 within the observed concentration ranged. The modified method also provided satisfactory results for sulfonylurea herbicides. The method was applied to the determination of residues of target pesticides in real samples. A total of 26 pesticides in 36 out of 98 tasted samples were observed. The highest concentration was observed for tricyclazole at 1.17 mg $kg^{-1}$ in brown rice. This pesticide in two brown rice samples exceeded their MRLs regulated for rice in republic of Korea. Except tricyclazole none of the observed pesticides' concentration was higher than their MRLs. The results reveal that the method is effectively applicable to routine analysis of residues of target pesticides in brown rice, barley and corn.

• Journal of the Mineralogical Society of Korea
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• v.15 no.4
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• pp.329-344
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• 2002

Mineralogical and chemical characterization of some domestic bentonites, such as quantitative XRD analysis, chemical leaching experiments, pH and CEC determinations, were done without any separation procedures to understand their relationships among mineral composition, characteristics, and cation exchange properties. XRD quantification results based on Rietveld method reveal that the bentonites contain totally more than 25 wt% of impurities, such as zeolites, opal-CT, and feldspars, in addition to montmorillonite ranging 30～75 wt%. Cation exchange properties of the zeolitic bentonites are deeply affected by the content of zeolites identified as clinoptilolite-heulandite series. Clinoptilolite is common in the silicic bentonites with lighter color. and occurs closely in association with opal-CT. Ca is mostly the dominant exchangeable cation, but some zeolitic bentonites have K as a major exchangeable cation, The values of cation exchange capacity (CEC) determined by Methylene Blue method are comparatively low and have roughly a linear relationship with the montmorillonite content of the bentonite, though the correlated data tend to be rather dispersed. Compared to this, the CEC determined by Ammonium Acetate method, i.e.‘Total CEC’, has much higher values (50～115 meq/100 g). The differences between those CEC values are much greater in zeolitic bentonites, which obviously indicates the CEC increase affected by zeolite. Other impurities such as opal-CT and feldspars seem to affect insignificantly on the CEC of bentonites. When dispersed in distilled water, the pH of bentonites roughly tends to increase up to 9.3 with increasing the alkali abundance, especially Na, in exchangeable cation composition. However, some bentonites exhibit lower pH (5～6) so as to regard as ‘acid clay’. This may be due to the presence of $H^{＋}$ in part as an exchangeable cation in the layer site of montmorillonite. All the works of this study ultimately suggest that an assesment of domestic bentonites in grade and quality should be accomplished through the quantitative XRD analysis and the ‘Total CEC’measurement.

• 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.46 no.9
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• pp.1091-1096
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• 2017

The aim of this study was the validation of a modified analytical method for determination of oxypaeoniflorin and paeoniflorin in Moutan Cortex Radicis extract. For validation of the analytical method, we modified established analytical methods and validated improvement. For validation, the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification of oxypaeoniflorin and paeoniflorin were measured by high performance liquid chromatography. The results show that the correlation coefficients of the calibration curve for oxypaeoniflorin and paeoniflorin were 1.0000 and 0.9998, respectively. The LOD for oxypaeoniflorin and paeoniflorin were $0.23{\mu}g/mL$ and $0.25{\mu}g/mL$, respectively. The inter-day and intra-day precision values of oxypaeoniflorin and paeoniflorin were 0.70~3.19% and 1.74~2.43%, and 0.32~0.92% and 0.62~2.28%, respectively. The inter-day and intra-day accuracies of oxypaeoniflorin and paeoniflorin were 98.33~102.11% and 97.72~118.12%, and 98.44~101.56% and 97.10~112.00%, respectively. Therefore, the analytical method was validated for the detection of oxypaeoniflorin and paeoniflorin in Moutan Cortex Radicis.