• Advances in materials Research
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• v.13 no.3
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• pp.233-241
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• 2024

Quantitative analysis of the Zingiber Officinale sample using subcritical water extraction (SWE) was developed employing High-Performance Liquid Chromatography (HPLC) to bolster the advancement of this innovative green extraction process. This research focuses on three principal ginger bioactive compounds: 6-gingerol, 6-shagoal, and 10-gingerol. Various stages were undertaken to establish the quantitative analysis method, encompassing the optimisation of HPLC operating conditions and the formulation of standard calibration curves, yielding individual compound equations. A robust correlation within the calibration curve was achieved, exhibiting an r² value of 0.9814 and an RSD of 5.00%. A simultaneous, swift, and dependable method was established with an injection time of 20 minutes and an 8-minute delay between injections, in contrast to the previous HPLC analysis requiring a 45-minute injection time for detecting and quantifying all components. Notably, no post-treatment was applied after the SWE process. This advancement allows for potential future online measurement of Zingiber Officinale bioactive compounds extracted using subcritical water extraction through this technology.

• The Korean Journal of Pesticide Science
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• v.17 no.4
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• pp.264-270
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• 2013

Imidacloprid is a systemic insecticide which act as an insect neurotoxin. It used for control of pest such as aphids and other sucking insects in fruits and vegetables. Systemic pesticides move inside a crop following absorption by the plant, and these were converted into a variety of metabolites. Sometimes these metabolites make a problem about safety of agricultural products. So a simultaneous determination method of pesticide and its metabolites is needed, to monitor their presence in agricultural product and study on the fate of pesticide in a plant. This study's aim is to investigate simultaneous analysis method of imidacloprid and its metabolites, imidacloprid guanidine, imidacloprid olefin, imidacloprid urea, and 6-chloronicotinic acid in red pepper using QuEChERS method and LC-MS/MS systems. QuEChERS method was modifed beacuase $MgSO_4$ salts decreased the recoveries of 6-chloronicotinic acid in extraction procedure. Imidacloprid and its metabolites were extracted by acetonitrile with 1% glacial acetic acid and the extracts were purified through QuEChERS with primary secondary amine (PSA) and $C_{18}$ and analyzed with LC-MS/MS in ESI positive mode. Standard calibration curves were made by matrix matched standards and their correlation coefficients were higher than 0.999. Recovery studies were carried out on spiked pepper blank sample at four concentration levels (0.01, 0.04 and 0.1, 0.4 mg/kg). The average recoveries of imidacloprid and its metabolites were in the range of 70~120% with < 20% RSD. This result indicated that the method using QuEChERS and LC-MS/MS was suitable for the simultaneous determination of imidacloprid and its metabolites in red pepper.

• Korean Journal of Food Science and Technology
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• v.51 no.6
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• pp.517-523
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• 2019

In this study, we investigated antioxidant capacity of 20 strawberry extract using the DPPH and ABTS assay and HPLC-DAD validation method. The total polyphenolic and flavonoids contents of 20 strawberry extracts were 22.77-107.61 mg TAE/100 g FW and 17.58-44.12 mg QE/100 g FW. The Aiberry and Elie star showed the highest total polyphenol and flavonoid contents, respectively. The DPPH radical scavenging activity of what was 1540.6-1124.0 μmol TEAC/100 g FW and Derunoka showed the highest activity. The ABTS radical scavenging activity was 6352.3-4592.3 μmol TEAC/100 g FW and FA23 showed the highest activity. The HPLC-DAD method for the quantitation of ellagic acid results showed high linearity in various concentration ranges, and the limit of detection was 2.35 μg/mL. The limit of quantification was 7.12 μg/mL. Relative standard deviation values from intra-and inter-day precision were less than 5.31%. Recovery rate at 10, 50, and 100 μg/mL, respectively, were 100.0-101.0% with relative standard deviation (RSD) values less than 5.30%. These results provide viable information for the validation of antioxidant capacity in strawberry fruits.

• Journal of Food Hygiene and Safety
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• v.26 no.1
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• pp.16-24
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• 2011

A method was established for the simultaneous determination of sugar alcohols, erythritol, xylitol, sorbitol, inositol, mannitol, maltitiol, lactitol and isomalt by High Performance Liquid Chromatography (HPLC). The sugar alcohols were converted into strong ultraviolet (UV)-absorbing derivatives with p-nitrobenzoyl chloride (PNBC). HPLC was performed on Imtakt Unison US-$C_18$ column, using acetonitrile: water (77:23) as a mobile phase and UV detection (260 nm). The calibration curves for all sugar alcohols tested were linear in the 10~200 mg/L range. The average recoveries of the sugar alcohols from three confectioneries spiked at 100 ppm of eight sugar alcohol standards ranged from 81.2 to 123.1% with relative standard deviations ranging fromo 0.2 to 4.9%. The limits of detection (LODs) were $0.5{\sim}8\;{\mu}g/L$ and the limits of quantification (LOQs) were $2{\sim}17\;{\mu}g/L$. Reproducibility of 8 sugar alcohols was 0.28~1.97 %RSD. The results of the analysis of confectioneries showed that 89 samples of 130 were detected and the sugar alcohols content of samples investigated varied between 0.4 and 693.7 g/kg. A method for the simultaneous determination of eight sugar alcohols will be used as basic data for control of sugar alcohols in confectioneries, and quality control in food manufacturing.

• Journal of Food Hygiene and Safety
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• v.20 no.4
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• pp.277-283
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• 2005

A plasticizer is a substance which is added to a material to improve its processability, flexibility and stratchability. Phthalates and adipates are the most frequently used plasticizers of poly(vinyl chloride) (PVC). However, they can migtate into food from PVC food packaging, and some of them are especially suspected as endocrine disruptors. In this study, Simultaneous analysis of 13 phthalates and 9 adipates were carried out by dual-column gas chromatography system equipped wi two FID detectors for rapid confirmation and quantification. The Proposed method was validated with > 0.993 of linearity in the ranges of 10-500 mg/l, < $3.5\%$ RSD of reproducability in 10 inter-days sample preparations, and > $98.1\%$ of recoveries for all the plasticizers. DEHA was detected in all the 3 PVC wraps at levels of 176.9-198.5mg/g. Among the 51 samples of PVC gaskets, the targeted plasticizers were detected in 41 samples. Of these plasticizer detected samples,40 contained DIDP at the levels of 157.3-374.7 mg/g and one contained DMP at the levels of 165.6 mg/g. Also, some plasticizers were detected in other packaging materials such as PET, PP, PE, Pulp. But it might be attributed to contamination in manufacturing.

• Journal of Korean Society for Atmospheric Environment
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• v.32 no.5
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• pp.501-512
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• 2016

The study evaluated methods to measure condensable fine particles in flue gases and measured particulate matter by fuel and material to get precise concentrations and quantities. As a result of the method evaluation, it is required to improve test methods for measuring Condensable Particulate Matter (CPM) emitted after the conventional Filterable Particulate Matter (FPM) measurement process. Relative Standard Deviation (RSD) based on the evaluated analysis process showed that RSD percentages of FPM and CPM were around 27.0~139.5%. As errors in the process of CPM measurement and analysis can be caused while separating and dehydrating organic and inorganic materials from condensed liquid samples, transporting samples, and titrating ammonium hydroxide in the sample, it is required to comply with the exact test procedures. As for characteristics of FPM and CPM concentrations, CPM had about 1.6~63 times higher concentrations than FPM, and CPM caused huge increase in PM mass concentrations. Also, emission concentrations and quantities varied according to the characteristics of each fuel, the size of emitting facilities, operational conditions of emitters, etc. PM in the flue gases mostly consisted of CPM (61~99%), and the result of organic/inorganic component analysis revealed that organic dusts accounted for 30~88%. High-efficiency prevention facilities also had high concentrations of CPM due to large amounts of $NO_x$, and the more fuels, the more inorganic dusts. As a result of comparison between emission coefficients by fuel and the EPA AP-42, FPM had lower result values compared to that in the US materials, and CPM had higher values than FPM. For the emission coefficients of the total PM (FPM+CPM) by industry, that of thermal power stations (bituminous coal) was 71.64 g/ton, and cement manufacturing facility (blended fuels) 18.90 g/ton. In order to estimate emission quantities and coefficients proper to the circumstances of air pollutant-emitting facilities in Korea, measurement data need to be calculated in stages by facility condition according to the CPM measurement method in the study. About 80% of PM in flue gases are CPM, and a half of which are organic dusts that are mostly unknown yet. For effective management and control of PM in flue gases, it is necessary to identify the current conditions through quantitative and qualitative analysis of harmful organic substances, and have more interest in and conduct studies on unknown materials' measurements and behaviors.

• The Korean Journal of Pesticide Science
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• v.18 no.4
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• pp.269-277
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• 2014

The multiclass pesticide multiresidue method for the simultaneous determination of diflubenzuron in agricultural products was conducted by using HPLC-UVD. The method was validated through the guidelines of linearity, specificity, limit of detection (LOD), limit of quantification (LOQ), accuracy and precision with pesticide-free spinach, Korean cabbage, eggplant, squash, sweet pepper, cucumber, Korean melon. The calibration curve of diflubenzuron was linear over the concentration range of 0.05-5 mg/kg with correlation coefficient of above 0.99999. The limit of detection and quantification was 0.008 and 0.02 mg/kg. Mean recoveries of diflubenzuron for each sample were 77.5-105.6%. Relative standard deviation (RSD) in recoveries were all less than 20%. The intra-day and inter-day precision (RSD) were 0.4-1.9% and 0.7-1.9%, respectively. The result of validation indicated that this method was accurate and rapid assay.

• Journal of Food Hygiene and Safety
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• v.31 no.2
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• pp.85-93
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• 2016

A rapid method using HPLC-MS/MS has been developed for quantitative determination of the metabolites of nitrofurans, namely 3-amino-2-oxazolidone (AOZ), 5-morpholinomethyl-3-amino-2-oxazolidinone (AMOZ), 1-ammino-hydantoin (AHD) and semicarbazide (SEM) in loach. The extraction procedure was founded on simultaneous acidic hydrolysis and derivatization using 2-nitrobenzaldehyde (2-NBA) for 1 hour at $50^{\circ}C$, followed by purification with liquid-liquid extraction. Recovery was evaluated by spiking standards into blank samples at three levels (0.5, 1.0 and $2.0{\mu}g/kg$), and the mean recovery was 75.1-108.1%. Precision values expressed as the relative standard deviation (%RSD) were ${\leq}8.7%$ and ${\leq}8.5%$ for intra-day and inter-day precision, respectively. Linearity was studied in the range of $0.2-20{\mu}g/Kg$ for NBAOZ, $0.8-20{\mu}g/Kg$ for NBAMOZ, $0.2-20{\mu}g/Kg$ for NBAHD, and $0.1-20{\mu}g/Kg$ for NBSEM, and the obtained coefficient correlations (r) were ${\geq}0.99$ for all compounds. Limits of detection (LODs) for the derivatized nitrofuran metabolites were established at $0.06{\mu}g/Kg$ for NBAOZ, $0.24{\mu}g/Kg$ for NBAMOZ, $0.06{\mu}g/Kg$ for NBAHD, and $0.03{\mu}g/Kg$ for NBSEM. Limits of quantification (LOQs) were established at $0.2{\mu}g/Kg$ for NBAOZ, $0.8{\mu}g/Kg$ for NBAMOZ, $0.2{\mu}g/Kg$ for NBAHD, and $0.1{\mu}g/Kg$ for NBSEM. This simplified rapid method for reducing the derivatization and hydrolysis times can be applied to the determination of nitro-furan residues in loach.

• 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.