• Journal of Food Hygiene and Safety
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• v.37 no.2
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• pp.39-45
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• 2022

This study aimed to investigate the validation and modify the analytical method to determine quercetin-3-𝑜-gentiobioside and isoquercitrin in Abelmoschus esculentus L. Moench for the standardization of ingredients in development of functional health products. The analytical method was validated based on the ICH (International Conference for Harmonization) guidelines to verify the reliability and validity there of on the specificity, linearity, accuracy, precision, detection limit and quantification limit. For the HPLC analysis method, the peak retention time of the index component of the standard solution and the peak retention time of the index component of A. esculentus L. Moench powder sample were consistent with the spectra thereof, confirming the specificity. The calibration curves of quercetin-3-𝑜-gentiobioside and isoquercitrin showed a linearity with a near-one correlation coefficient (0.9999 and 0.9999), indicating the high suitability thereof for the analysis. A. esculentus L. Moench powder sample of a known concentration were prepared with low, medium, and high concentrations of standard substances and were calculated for the precision and accuracy. The precision of quercetin-3-𝑜-gentiobioside and isoquercitrin was confirmed for intra-day and daily. As a result, the intra-day precision was found to be 0.50-1.48% and 0.77-2.87%, and the daily precision to be 0.07-3.37% and 0.58-1.37%, implying an excellent precision at level below 5%. As a result of accuracy measurement, the intra-day accuracy of quercetin-3-𝑜-gentiobioside and isoquercitrin was found to be 104.87-109.64% and the daily accuracy thereof was found to be 106.85-109.06%, reflecting high level of accuracy. The detection limits of quercetin-3-𝑜-gentiobioside and isoquercitrin were 0.24 ㎍/mL and 0.16 ㎍/mL, respectively, whereas the quantitation limits were 0.71 ㎍/mL and 0.49 ㎍/mL, confirming that detection was valid at the low concentrations as well. From the analysis, the established analytical method was proven to be excellent with high level of results from the verification on the specificity, linearity, precision, accuracy, detection limit and quantitation limit thereof. In addition, as a result of analyzing the content of A. esculentus L. Moench powder samples using a validated analytical method, quercetin-3-𝑜-gentiobioside was analyzed to contain 1.49±0.01 mg/dry weight g, while isoquercitrin contained 1.39±0.01 mg/dry weight g. The study was conducted to verify that the simultaneous analysis on quercetin-3-𝑜-gentiobioside and isoquercitrin, the indicators of A. esculentus L. Moench, is a scientifically reliable and suitable analytical method.

• The Korean Journal of Pesticide Science
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• v.12 no.4
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• pp.323-334
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• 2008

This experiment was carried out to analyze for pesticide residues in 17 different types of the special of geographical indication. We purchased 3 cereal grains, nuts and seeds, 3 fruits, 8 vegetables, mushrooms and other plants (Korean medicines) mainly at the agricultural cooperative's joints markets. Total 209 pesticides including multi-analysed pesticides (204) and single-analysed pesticides (5 ; acephate, methamidophos, monocrotophos, omethoate, vamidothion) were analysed with a GC/MS/MS, an HPLC/UVD (PDA) and a GC/FPD. No. 83 method and single-analysed method (Screening of multi-pesticide residue in the special products of geographical indication) of Korea Food Code was selected for validation in recovery and interferences of matrice. The results were as follows: among the selected 17 the special products, the residual pesticides were detected in 8 types of the special products (40 in 302 samples, detection ratio; 13.2%). All of the samples were not detected over MRLs, but tebuconazole, procymidone and isoprothioran were detected with considerable high frequency. These results could be used as KFDA official methods for the analysis of pesticide residues in foods and reference data will be provided to the related institutions.

• The Korean Journal of Pesticide Science
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• v.16 no.3
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• pp.195-201
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• 2012

We tested for pesticide residues in 124 samples of 22 different items of imported fruits circulated in Gyeonggido. Total 218 pesticides were analyzed by multi-residue method using gas chromatography/nitrogen phosphorus detector-electron capture detector (GC/NPD-ECD), time of flight/mass spectrometer (TOF/MS), ultra performance liquid chromatography/photo diode array (UPLC/PDA), high performance liquid chromatography/fluorescence detector (HPLC/FLD) and mass spectrometer (LC/MS/MS). The pesticides were detected in 18 fruits samples, ranging 0.003~0.3 mg/kg and no samples had violative residue. The separation test to 14 sample pesticides detected was conducted to monitor the current status of pesticide residues according to the partial characteristic. The pesticides were detected in 14 peels ranging 0.03~1.5 mg/kg and 2 fleshes in less than detection limits. These results indicate that imported fruits are safe when the human takes normally but even the small amount of pesticides is harmful when the human takes it in a prolonged period. Therefore, the pesticide residual amounts of imported friuts should be constantly monitored for food safety.

• Journal of Food Hygiene and Safety
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• v.31 no.1
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• pp.36-41
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• 2016

Ochratoxin A and aflatoxin may be detected from naturally fermented foods due to the contamination of the mycotoxin-producing molds or un-prudential use of the mycotoxin producing starter strains during the fermentation. This study was carried out to analyze the production of ochratoxin A and aflatoxin under the various environmental conditions. For the experiment, the effects of different temperature, culture media, and fermentation time on the production of ochratoxin A by Aspergillus usamii KFRI 999 and A. awamori KFRI 983 were analyzed. Additionally, the production of aflatoxin was assessed under the various temperature, initial pH, fermentation time and culture media during fermentation by A. flavus KACC 41403 and A. oryzae KACC 46471. The levels of ochratoxin A and aflatoxin were analyzed by HPLC. The result showed that the production of mycotoxin was greatly affected by the fermentation temperature. A. oryzae KACC 46471 did not produce aflatoxin. All of the mycotoxin producing strains showed the highest level of mycotoxin at $30^{\circ}C$. A. awamori KFRI 983 showed the lowest level of ochratoxin A in PDA media among the experimental medium. The results of the present study may be useful for the reduction of ochratoxin A and aflatoxin in various foods.

• Journal of Food Hygiene and Safety
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• v.29 no.2
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• pp.92-98
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• 2014

The safety of fake anti-impotence drugs (fake Viagra : 26 samples, fake Cialis : 25 samples) distributed in Gyeonggi province was studied by monitoring the concentrations of anti-impotence pharmaceutical ingredient and their analogues. The concentrations of anti-impotence pharmaceutical ingredient 4 specis and their analogues 17 specis were estimated using by HPLC/PDA, LC-MS/MS. The range of concentration of sildenafil in fake viagra was 40~199 mg/tablet, among them the portion of the concentrations of sildenafil over 150 mg/tablet exceeded 65%. 3 cases in tested samples contained sildenafil and tadalafil. The range of concentration of sildenafil in fake cialis was 102~249 mg/tablet, among them the portion of the concentrations of sildenafil over 150 mg/tablet exceeded 88%. One case in tested samples contained demethylhongdenafil (90 mg/tablet). These results indicate that there were many fake anti-impotence drug contained high level of anti-impotence pharmaceutical ingredients, a sustainable monitoring and the blocked distribution of fake anti-impotence drugs recommended.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.22 no.4
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• pp.483-492
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• 2021

Agastachis Herba (AH) to treat anorexia and nausea and its antidiabetic efficacy was recently reported. This study examined the antioxidant activities and chemical constituents of AH and predicted the target proteins of each compound using in silico approaches. The results showed that EC50 values of AH methanol extract for DPPH and ABTS radical scavenging were 78.6 ㎍/mL and 31.0 ㎍/mL, respectively. Compared to the EC50 values of ascorbic acid (9.9 ㎍/mL, 5.2 ㎍/mL), the AH methanol extract possessed excellent antioxidant activities. Rosmarinic acid, tilianin, agastachoside, and acetin were confirmed as the major compounds of extracts by qualitative analysis performed with HPLC-PDA-MS/MS. The antidiabetic target proteins of these compounds were predicted by applying a structural similarity and inverse docking methodology using a DIA-DB server. The resulting target proteins were PPAR-γ, DPP IV, glucokinase, α-glucosidase, SGLT2, aldose reductase, and corticosteroid 11-beta-dehydrogenase, some of which have already been proven experimentally as target proteins. Therefore, the in silico methods can be considered valid. Finally, AH were extracted with various solvents to determine the optimal conditions for the extraction of active components. Methanol among organic solvents and 80% ethanol in ethanol-water mixtures were identified as the most effective solvent for the extraction.

• Journal of Food Hygiene and Safety
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• v.37 no.1
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• pp.1-8
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• 2022

In this study, the pesticide residues in 106 commercial cereal grains were monitored from February to July 2021. For the investigation, 40 domestic and 66 imported products from large, small-to-medium sized offline and online distribution channels, were collected and analyzed by using the multiresidue method for 341 pesticides on GC/ECD, GC/NPD, GC/MSMS, UPLC/PDA, HPLC/FLD, LC/MSMS. Pesticides were detected in total of 8 samples (7.5%), of which one was from big box retailers, two from small and medium-sized distribution stores, and five from online shopping mall. Five (4.7%) samples were found to have pesticide residues greater than the maximum residue limits (MRLs). The detected pesticides in kidney beans (1 case), mung beans (6 cases), and sorghum (1 case), were MGK-264, chlorpyrifos, thiamethoxam, malathion, piperonyl butoxide, and pirimiphos-methyl. Specifically, an excessive amount of thiamethoxam was found from the imported mung bean (5 cases).

• The Korea Journal of Herbology
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• v.28 no.6
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• pp.47-51
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• 2013

Objectives : The Illicii Veri Fructus was not only traditional medicine but also food in Asia. The aim of this study was selection of optimum solvent in the fruit of Illicii Veri Fructus because an appropriate solvent affect a medicinal effect. Methods : Illicii Veri Fructus was carried out ultrasonic-assisted extraction as various solvents. Two main compounds, p-anisaldehyde and anethole, were successfully analyzed by high performance liquid chromatography-photodiode array detector (HPLC-PDA) and carried out method validation according to ICH guideline. The optimum solvent selected by comparing with yields of two main ingredients. Results : The p-anisaldehyde and anethole were detected at approximately 8.0 min and 19.8 min, respectively. It was all below 5.0% that RSD of retention time and peak area for two main peaks. Calibration curves of two compounds were good linearity as $R^2$ >0.9999. All of the precisions and accuracy were good intra-day and inter-day as below 5.0% RSD. Limited of detection (LOD) of p-anisaldehyde and anethole were analyzed as $0.134{\mu}g/mL$ and $4.286{\mu}g$, respectively. Limited of quantification (LOQ) of two compounds were $0.407{\mu}g$ and $12.989{\mu}g$, respectively. As a result of this study, p-anisladehyde was detected as 0.209 ~ 0.467%, however anethole was not detected in the distilled water. Conclusions : Anethole was main component as 5.329 ~ 6.815% except for water extraction. Methanol extraction among various solvents was detected the highest contents of p-anisaldehyde and anethole as 0.467(${\pm}0.008$)% and 6.815(${\pm}0.220$)%, respectively.

• Journal of Society of Preventive Korean Medicine
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• v.17 no.3
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• pp.165-176
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• 2013

Objective : The purpose of this study was to establish the simultaneous analysis for six compounds in Gumiganghwal-tang (GMGHT, Jiuweiqianghuo-tang) and to investigate the anti-atherosclerotic effects of GMGHT in vitro. Methods : The column for separation of six compounds was used Luna $C_{18}$ column and maintained at $40^{\circ}C$. The mobile phase for gradient elution consisted of two solvent systems, 1.0% acetic acid in water and 1.0% acetic acid in acetonitrile. The analysis was carried out at a flow rate of 1.0 mL/min with pothodiode array (PDA) detection at 254, 280, and 320 nm. The injection volume was 10 ${\mu}L$. The antioxidant activities of GMGHT were evaluated by measuring free radical scavenging activities on 2,2'-Azinobis-3-ethyl-benzothiazoline-6-sulfonic acid (ABTS) and 1-1-diphenyl-2-picrylhydrazyl (DPPH). The inhibitory effects on low-density lipoprotein (LDL) oxidation were evaluated by the formation of thiobarbituric acid relative substances (TBARS), relative electrophoretic mobility (REM), and fragmentation of apolipoprotein B (ApoB)-100. Results : Calibration curves were acquired with $r^2{\geq}0.9998$. The contents of liquiritin, ferulic acid, baicalin, baicalein, glycyrrhizin, and wogonin in GMGHT were 1.784, 1.693, 37.899, 0.258, 1.869, and 0.034 mg/g, respectively. The GMGHT showed the radical scavenging activity in a dose-dependent manner. The concentration required for 50% reduction ($RC_{50}$) against ABTS and DPPH radicals were 72.51 ${\mu}g/mL$ and 128.49 ${\mu}g/mL$. Furthermore, GMGHT reduced the oxidation properties of LDL induced by $CuSO_4$. Conclusion : HPLC-PDA is considered as an available and convenient method for quality control and standardization of GMGH and GMGHT has potentials on anti-atherosclerosis by anti-oxidative effect and suppressive effect on LDL oxidation.

• Journal of Sasang Constitutional Medicine
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• v.25 no.1
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• pp.51-61
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• 2013

Objectives We performed the simultaneous analysis for three compounds in Cheongsimyeonja-tang (CSYJT) and evaluated its anti-obesity effect. Methods The column for separation of three compounds was used Gemini $C_{18}$ column and maintained at $40^{\circ}C$. The mobile phase for gradient elution consisted of two solvent systems. The analysis was carried out at a flow rate of 1.0 mL/min with PDA detection at 275 nm. The injection volume was $10{\mu}L$. 3T3-L1 preadipocytes were differentiated into adipocytes by adding insulin, dexamethasone and 3-isobutyl-1-methylxanthine (IBMX) for 8 days in the absence or presence of CSYJT. Anti-obesity effects of CSYJT were evaluated by Oil Red O staining, glycerol-3-phosphate dehydrogenase (GPDH) activity, triglyceride contents, and leptin production. Results Calibration curves were acquired with $r^2$ >0.9999. The contents of baicalin, wogonoside and baicalein in CSYJT were 14.54-14.65 mg/g, 5.24-5.27 mg/g and 0.01-0.02 mg/g, respectively. CSYJT showed inhibitory effect on lipid accumulation and GPDH activity in the differentiated 3T3-L1 cells. Furthermore, CSYJT significantly decreased contents of triglyceride and leptin production in 3T3-L1 adipocytes. Conclusions These results will be helpful to improve quality control and anti-obesity effect of Taeeumin CSYJT.