• Journal of Food Hygiene and Safety
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• v.26 no.2
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• pp.125-141
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• 2011

Melamine has raised international concerns for its catastrophic health effects from tainted infant formula. This report concerns the developmental validation of a sensitive HPLC/MS/MS and GC/MS methods about melamine and cyanuric acid in human urine and serum. Analytical detection ranges of LC/MS was from 0.2 to 5.0 ng/mL and 2.0 to 60.0 ng/mL about melamine and cyanuric acid, respectively. The limits of quantification and confirmation are 0.2 ng/mL for both analytes in human urine and serum by LC/MS/MS. The range of recovery was 91.6%, and 107.6% for cyanuric acid and melamine in urine, respectively. The range of precision coefficient variation was from 2.0%, to 11.8% for cyanuric acid and melamine in urine. The range of recovery was from 94.9%, to 119.0% about cyanuric acid and melamine in serum, respectively. The range of precision coefficient variation from was 3.7%, and 13.5% about cyanuric acid and melamine in serum. Analytical detection ranges of GC/MS were 5.0 to 100.0 ng/mL about melamine and cyanuric acid, respectively. The limits of quantification and confirmation are 5.0 ng/mL for both analytes in human urine and serum by GC/MS. The range of recovery was from 83.7%, to 114.5% for cyanuric acid and melamine in urine, respectively. The range of precision coefficient variation was 3.5%, and 10.7% for cyanuric acid and melamine in urine. The range of recovery was 94.4%, and 110.7% for cyanuric acid and melamine in serum, respectively. The range of precision coefficient variation from was 3.9%, and 13.8% for cyanuric acid and melamine in serum. Several changes were taken to optimize performance by this method.

• Journal of Food Hygiene and Safety
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• v.24 no.1
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• pp.56-62
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• 2009

Patulin, a mycotoxin mainly produced by Penicillium and Aspergillus, is found in various foods. In the present, a maximum acceptable level for patulin is established at $50{\mu}g/kg(ppb)$ in apple juices and apple concentrates in Korea. But patulin may be detected in foods produced with other fruits. In the present study, patulin contamination was analyzed in 520 samples of fruit juices and beverages, and 50 samples of fruit juice concentrates. High performance liquid chromatography(HPLC) was applied to quantitatively analyze patulin levels in samples and liquid chromatography-mass spectrometry(LC/MS/MS) was used to remove false positive results. The results showed that three samples of 520 fruit juices and beverages and five samples of 50 fruit juice concentrates were contaminated by patulin, $9.8-18.0{\mu}g/kg$ and $4.7-18.2{\mu}g/kg$ respectively. Contaminated samples were produced with apple, orange or pear. This indicates that it is necessary to extend the regulatory range of patulin. In the other hands, the present study confirmed the effectiveness of LC/MS/MS analytical method to remove false positive results.

• Journal of Food Hygiene and Safety
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• v.20 no.3
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• pp.141-146
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• 2005

A simple and sensitive analysis method based on reverse phase (RP) HPLC with UV detector was developed for simultaneous determination of chlorophyll a and b, pheophorbide a and $\beta-Carotene$ in Chlorella and Spirulina products. For added concentration $(50\;\mug/ml)$ of chlorophyll a and b, pheophorbide a and $\beta-Carotene$, recoveries of those were 70.3, 71.6, 60.1 and $90.5\%$, respectively, with relative standard deviations of 2.8,6.0, 10.6 and $10.4\%$. Limit of detection and quantification had ranges of $0.1\sim1.0\;\mug/ml$ and $0.2\sim2.0\;\mug/ml$, respectively. Calibration curve was linear with correlation coefficient of 0.995 for chlorophyll a and b, pheophorbide a and $\beta-Carotene$. Results of simultaneous determination in Chlorella and Spirulina products were showed ranges of $121.g\sim543.0\;\mug/ml$ for chlorophyll a,$0.6\sim160.0\;\mug/ml$ for chlorophyll b, $19.2\sim60.3\;\mug/ml$ for pheophorbide a and $383.6\sim1713.7\;\mug/ml$ for $\beta-Carotene$, respectively. Chlorophyll b contents in Chlorella products were detected above 30 times level to those in Spirulina products. $\beta-Carotene$ contents in Spirulina products were detected 2.7 times level to those in Chlorella products.

• The Korean Journal of Pesticide Science
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• v.14 no.4
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• pp.381-393
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• 2010

In order to monitor the residual characteristics of the pesticides in leafy vegetables selling at wholesale markets and traditional markets in Cheongju, a total of 180 samples of 15 leafy vegetables, such as broccoli, celery, chard, chicory, Chinese vegetable, Chwinamul, crown daisy, Korean cabbage, leek, lettuce, perilla leaves, Shinsuncho, spinach, welsh onion and young radish, were purchased from the wholesale markets and traditional markets in June and August in 2010 and the pesticide residues in them were analyzed by multiresidue analysis method using GLC, HPLC and GC-MSD. Seven pesticides were detected from 12 samples out of total 180 samples collected, representing detection rate was 6.7%. In case of the samples collected from markets in June, four pesticides including tefluthrin were detected from six samples and in case of the samples collected from markets in August, three pesticides including pendimethalin were detected from three samples. The MRL-exceeding rate of pesticides detected from leafy vegetables was 0.6%. The pesticide exceeded its MRL was azoxystrobin detected from crown daisy and many pesticides were not registered to the crops, excepting that azoxystrobin detected from Chwinamul and tefluthrin from leek. Estimated daily intakes (EDIs) of the pesticides detected from leafy vegetables were less than 7% of their acceptable daily intakes (ADIs), representing that residue levels of the pesticides detected were evaluated as safe.

• Journal of Pharmaceutical Investigation
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• v.34 no.1
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• pp.49-55
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• 2004

To develop a aceclofenac soft capsule, four preparations with various solubilizers were prepared and their dissolution test was carried out. Among four preparations tested, a preparation with ethanolamine was selected as a formula of aceclofenac soft capsule (Clanza $S^{TM}$), since it showed the fastεst dissolution rate. Bioequivalence of aceclofenac tablet, $Airtal^{TM}$ (Dae-Woong Pharmaceutical Co., Ltd.) and aceclofenac soft capsule, Clanza $S^{TM}$ (Korea United Pharmaceutical Co., Ltd.) was evaluated according to the guideline of KA Fourteen normal male volunteers (age 20 - 25 years old) were divided into two groups and a randomized $2{\times}2$ cross-over study was employed. After oral administration of one tablet or capsule containing 100 mg of aceclofenac, blood was taken at predetermined time intervals and the concentration of aceclofenac in plasma was determined with an HPLC method under UV detector The pharmacokinetic parameters ($C_{max}$ and $AUC_t$) were calculated and ANOVA was utilized for the statistical analysis of parameters using logarithmetically transformed $AUC_t$, $C_{max}$ and $T_{max}$. The results showed that the differences in $AUC_t$, $C_{max}$ and $T_{max}$ between Aral tablet and Clanza soft capsule were 2.89%, 0.18% and 43.0%, respectively. There were no sequence effects between two formulations in these parameters. The 90% confidence intervals using logarithmically transformed data were within the acceptance range of log(0.8) to log(15) (e.g. log(0.81) -log(1.23) ad log(0.89) -log(1.4)) fo $AUC_t$ and $C_{max}$, respectively. Thus, the criteria of the KFDA guidelines for the equivalence was satisfied, indicating that Clanza $S^{TM}$ soft capsule is bioequivalent to$Airtal^{TM}$ tablet.

• Journal of Pharmaceutical Investigation
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• v.35 no.3
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• pp.179-185
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• 2005

Acebrophylline is a compound produced by salifying ambroxol with theophylline-7 -acetic acid. After acebrophylline administration, the salt splits into these two components which feature a peculiar pharmacokinetic behavior, an adequate ambroxol and a low theophylline-7-acetic acid serum levels. The purpose of the present study was to evaluate the bioequivalence of two acebrophylline capsules, Surfolase (Hyundai Pharm. lnd. Co., Ltd.) and Burophil (Kuhnil Pharm. Co., Ltd.), according to the guidelines of the Korea Food and Drug Administration (KFDA). The release of ambroxol from the two acebrophylline formulations in vitro was tested using KP VIII Apparatus II method with various dissolution media (pH 1.2, 4.0, 6.8 buffer solution and water). Twenty eight healthy male subjects, $23.25{\pm}1.43$ years in age and $64.82{\pm}6.77$ kg in body weight, were divided into two groups and a randomized $2{\times}2$ cross-over study was employed. After two capsules containing 100 mg as acebrophylline were orally administered, blood was taken at predetermined time intervals and the concentrations of ambroxol in serum were determined using HPLC with electrochemical detector (ECD). The dissolution profiles of two formulations were similar at all dissolution media. In addition, the pharmacokinetic parameters such as $AUC_t$, $C_{max}$ and $T_{max}$ were calculated and ANOVA test was utilized for the statistical analysis of the parameters using logarithmically transformed $AUC_t$, $C_{max}$ and untransformed $T_{max}$. The results showed that the differences between two formulations based on the reference drug Surfolase, were -1.64, -3.33 and -0.92% for $AUC_t$, $C_{max}$ and $T_{max}$, respectively. There were no sequence effects between two formulations in these parameters. The 90% confidence intervals using logarithmically transformed data were within the acceptance range of log 0.8 to log 1.25 $(e.g., \;log\;0.93{\sim}log\;1.05\;and\;log\;0.88{\sim}log\;1.05$ for $AUC_t$, and $C_{max}$, respectively). Thus, the criteria of the KFDA bioequivalence guideline were satisfied, indicating Burophil capsule was bioequivalent to Surfolase capsule.

• Journal of Pharmaceutical Investigation
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• v.36 no.3
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• pp.209-215
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• 2006

Zaltoprofen, (2-(10,11-dihydro-10-oxodibenzo[b,f]thiepin-2-yl)propionic acid) is an NSAID with powerful anti-inflammatory effects as well as an analgesic action on inflammatory pain. The purpose of the present study was to evaluate the bioequivalence of two zaltoprofen tablets, $Soleton^{\circledR}$ (CJ Corp.) and SCD Zaltoprofen (Samchundang Pharmaceutical Co., Ltd.), according to the guidelines of the Korea Food and Drug Administration (KFDA). The release of zaltoprofen from the two zatoprofen formulations in vitro was tested using KP Vlll Apparatus ll method with various dissolution media. Twenty six healthy male subjects, $23.2{\pm}2.26$ years in age and$64.7{\pm}8.08$ kg in body weight, were divided into two groups and a randomized $2{\times}2$ cross-over study was employed. After a single tablet containing 80 mg as zaltoprofen was orally administered, blood samples were taken at predetermined time intervals and the concentrations of zaltoprofen in serum were determined using HPLC with UV detector. The dissolution profiles of two formulations were similar in all tested dissolution media. The pharmacokinetic parameters such as $AUC_t$, $C_{max}$ and $T_{max}$ were calculated, and ANOVA test was utilized for the statistical analysis of the parameters using logarithmically transformed $AUC_t$, $C_{max}$ and untransformed $T_{max}$. The results showed that the differences between two formulations based on the reference drug, $Soleton^{\circledR}$ were 6.33, 5.91 and 17.7% for $AUC_t$, $C_{max}$ and untransformed $T_{max}$, respectively. There were no sequence effects between two formulations in these parameters. The 90% confidence intervals using logarithmically transformed data were within the acceptance range of log 0.8 to log 1.25 (e.g.,log $1.01{\sim}1og\;1.11$ and log $0.928{\sim}1og\;1.18$ for $AUC_t$ and $C_{max}$, respectively). Thus, the criteria of the KFDA bioequivalence guideline were satisfied, indicating SCD Zaltoprofen tablet was bioequivalent to $Soleton^{\circledR}$ tablet.

• The Korean Journal of Pesticide Science
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• v.15 no.2
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• pp.114-124
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• 2011

The characteristics of pesticide residues by multiresidue analysis method using GC, HPLC and GC-MSD were examined for 18,069 numbers of 91 kinds of vegetables in Seoul from 2007 to 2009. Detection rates of pesticide residues were 11.2% in 2007, 8.5% in 2008 and 12.0% in 2009, respectively, and the excess rates of Maximum Residue Limits (MRLs) showed a declining tendency as 4.6% in 2007, 2.8% in 2008 and 2.1% in 2009, respectively. The pesticides exceeding MRLs were 43 ingredients in 2007, 30 ingredients in 2008 and 36 ingredients in 2009, respectively. The frequencies of pesticides exceeding MRLs were 71 of azoxystrobin in 2007, 29 of procymidone in 2008, 24 of endosulfan in 2009, respectively. The excess rate of mustard green for MRLs in comparison with sample numbers was the highest among vegetables analyzed more than 10 cases each year. As a result of comparing annually pesticide residues about pesticide ingredients showed high frequency rates for pesticide detection, there was a statistical significance for the detection quantities of diazinon, endosulfan, paclobutrazol and procymidone.

• Journal of Sericultural and Entomological Science
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• v.47 no.2
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• pp.51-55
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• 2005

Resveratrol is naturally occurring phytoalexin compounds produced by grape berries, peanuts, and their products in response to stress such as fungal infection, heavy metal ions or UV irradiation. The objective of this study was to develope a reliable high performance liquid chromatographic (HPLC) method for the quantitative determination of trans-resveratrol in mulberry fruit. Samples were extracted in 80% MeOH and filtered with $0.45{\mu}m$ syringe filter. The transresveratrol was separated Waters $C_{18}$ column, using a mobile phase containing 0.025% trifluroacetic acid in 5% acetonitril and 0.035% trifluroacetic acid in 50% acetonitril, detected by photodiode array detector (PDA) at 254 nm and the flow rate was 1ml/min. Under this analytical condition, the mean content of mulberry fruits (fifty varieties) was $777.3{\pm}585.9ppm$. Among the tested samples, 'Mansaengbaekpinosang (II)' was the highest level in 3450.6 ppm. However four accessions including 'Gukbu', 'Sabangso (I)', 'Simseol' and yield mulberry fruit were not able to detected. Eight suitable varieties selected for the production of fruit were 'Jeolgokchosaeng (Chungbuk)' 777.8 ppm, 'Dangsang 7' 771.1 ppm, 'Jangsosang' 133.9 ppm, 'Susungppong' 31.1 ppm, 'Suwonnosang' 639.7 ppm, 'Palcheongsipyung' 1475.9 ppm, 'Kangsun' 864.0 ppm, and 'Jukcheonchosaeng' 1458.5 ppm. 'Daesungppong' which was the first authorized variety for the production of mulberry fruit was 1236.7 ppm. In conclusion, these results suggest that mulberry including fruit and leaf may a good new resource for resveratrol production.

• Applied Chemistry for Engineering
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• v.29 no.4
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• pp.452-460
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• 2018

This study was conducted to investigate the physiological activities of Houttuynia cordata extracts and fractions. H. cordata extracts were extracted with 50% ethanol and the ethyl acetate fractions were obtained from the extracts. Minimum inhibitory concentration (MIC) values of the ethyl acetate fraction for S. aureus and B. subtilis were $78{\mu}g/mL$ and $312{\mu}g/mL$, respectively, indicating the high activity against gram-positive bacteria. The free radical scavenging activity ($FSC_{50}$) for 1,1-diphenyl-2-picrylhydrazyl (DPPH) was higher in the ethyl acetate fraction with $12.00{\mu}g/mL$ compared to that of $27.15{\mu}g/mL$ for 50% ethanol extract. The total antioxidant activity ($OSC_{50}$) values for reactive oxygen species (ROS) produced in $Fe^{3+}-EDTA/H_2O_2$ system by a luminol-dependent chemiluminescence method were 2.91 and $0.983{\mu}g/ml$ for the 50% ethanol extract and ethyl acetate fraction, respectively. To investigate cellular protective effects on the HaCaT cell, the intracellular ROS scavenging activity was measured after UVB irradiation and the ethyl acetate fraction of H. cordata showed the activity in a concentration-dependent from $1.6{\mu}g/mL$ and a reduction rate of 54.3% at a maximum concentration of $12.5{\mu}g/mL$. Also, HaCaT cell protective effect against $H_2O_2$-mediated decreased the cell viability of the ethyl acetate fraction of H. cordata which significantly increased the cell viability from $0.8{\mu}g/mL$ and the maximum cell viability showed 86.9%. The ethyl acetate fraction of the H. cordata extracts was analyzed by TLC and HPLC. As a result, quercitrin, isoquercitrin, hyperoside, chlorogenic acid, neochlorogenic acid, cryptochlorogenic acid, rutin and afzelin were identified. From the above results, it was suggested that the extracts and fractions of H. cordata have a potential to be applied in the field of cosmetics as a natural antioxidant/preservative capable of protecting the cell membrane from the oxidative stress by eliminating ROS and exhibiting the antimicrobial effect.