• The Korean Journal of Food And Nutrition
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• v.36 no.2
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• pp.93-102
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• 2023

Centella asiatica (C. asiatica) has been widely used in food, cosmetics, and pharmaceutical industry as a functional material. In a previous study, we have investigated not only pharmacological effects such as antioxidative and anti-inflammatory effects, but also analyzed various functional ingredients. In this study, triterpenoids were analyzed using HPLC-DAD to determine marker compounds among functional ingredients. When triterpenoids were analyzed, asiaticoside from C. asiatica was determined as an optimal marker compound. Next, specificity, linearity, limited of detection (LOD), limited of quantification (LOQ), precision, accuracy, and range were evaluated using HPLC-DAD to determine asiaticoside contents in C. asiatica juice and extracts. The specificity was elucidated by chromatogram and retention time using an established analytical method. The coefficient of correlation obtained was 0.9996. LOD was 4.99 ㎍/mL and LOQ was 15.12 ㎍/mL. Intra- and inter-day precision of asiaticoside were determined to be 0.48~1.68% and 0.08~1.09%, respectively. Furthermore, the recovery rate of asiaticoside was 98.88% and the analytical range of Field-70E was determined to be 0.625~10 mg/mL. As a results of evaluating ABTS, DPPH, and FRAP antioxidative effect, Field-70E showed potent antioxidant activities. Results of this study could be used as basic data for quality standardization of C. astiatica juice and extracts.

• Analytical Science and Technology
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• v.22 no.6
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• pp.514-518
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• 2009

Coenzyme $Q_{10}$($CoQ_{10}$), a vitamin E-like substance, represents a components of the complex antioxidant system of the human organism. $CoQ_{10}$ levels in human plasma were determined by high performance liquid chromatography (HPLC) with UV detection. It was dissociated from lipoproteins by methanol and extracted into n-hexane with liquid-liquid extraction procedure, after centrifugation, the supernatant was dried under nitrogen gas stream. The residue was dissolved in the absolute ethanol. Determination of $CoQ_{10}$ was performed on a $C_{18}$ reversed-phase analytical column with ultraviolet detection at 275 nm and the mobile phase containing 15% (v/v) ethanol in methanol at a flow rate of 1.7 mL/min. The low limit of quantitation was 0.02 mg/L (S/N=10), the linearity between the concentration and peak height is from 0.1 to 2.0 mg/L. Twenty-four randomly selected plasma samples from apparently healthy, 27 to 44 year old individuals (males and females) were analyzed for total $CoQ_{10}$. The average level in these subjects was $0.62{\pm}0.13mg/L$ with the range of 0.41-0.98 mg/L. This method has a specific and a sufficient limit of quantitation (LOQ) for analysis of $CoQ_{10}$ in human plasma in both a clinical study and research at laboratories.

• Analytical Science and Technology
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• v.21 no.6
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• pp.535-542
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• 2008

A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed for the determination and confirmation of clenbuterol in bovine muscle and milk. Clenbuterol and clenbuterol-D9 using as an internal standard in samples were extracted with ethyl acetate after hydrolysis and evaporated to dryness. The extracts were dissolved in 20% methanol and cleaned using HLB solid-phase extraction cartridge. The analytes were detected by LC-ESI/MS/MS on a $C_{18}$ column. Mass spectral acquisition was done in selected reaction monitoring (SRM) in positive ion mode to provide a high degree of sensitivity. Using MS/MS with SRM mode, the transitions (precursor to product) monitored were m/z 277${\rightarrow}$203 for clenbuterol, and m/z 286${\rightarrow}$204 for internal standard. The limits of quantitation (LOQ) and mean recoveries of clenbuterol in bovine muscle were $0.2{\mu}g/kg$ and 84.3~91.1%, respectively. The LOQ and mean recoveries in milk were $0.05{\mu}g/kg$ and 87.7~98.3%, respectively.

• Journal of Food Hygiene and Safety
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• v.38 no.3
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• pp.89-98
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• 2023

Currently, no guidelines exist regarding the maximum residues of pesticides in edible oil which is a processed food commonly consumed in Korea. This lack of guidelines hinders the evaluation of the safety of edible oil in terms of pesticide contamination. In this study, an analysis method based on heat distillation and GC-MS/MS was established by optimizing the extraction and purification procedure for 68 pesticides. Important variables in the thermal distillation procedure included heating temperature and time, and we found the nitrogen flow rate as a mobile phase and the type of dissolving solvent were not considerably affected. The determination coefficient (R²) of the residual pesticide was 0.99 or higher, and the quantitative limit (LOQ) was 0.01-0.02 mg/L. The average recovery rate (n=5) was 66.1-120.0% and the relative standard deviation was lower than ±10% when 68 pesticides were spiked at concentrations of 0.01-0.02, 0.1, and 0.5 mg/L. In addition, the within-laboratory precision was less than ±11%, meeting the Korea Food and Drug Safety Evaluation Institute's Guidelines on Standard Procedures for Preparing Food Testing Methods (2016). Therefore, the test method developed in this study can be used as a test method for managing the safety of the residual pesticide concentration in edible oil.

• Bulletin of the Korean Chemical Society
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• v.31 no.5
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• pp.1192-1198
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• 2010

Pharmaceuticals and personal care products (PPCPs) are emerging contaminants in the aquatic environment. Many pharmaceuticals are not completely removed during wastewater treatment, leading to their presence in wastewater treatment effluents, rivers, lakes, and ground water. Here, we developed analytical methods for monitoring ten pharmaceuticals from surface water by LC/ESI-MS/MS. For sample clean-up and extraction, MCX (mixed cation exchange) and HLB (hydrophilic-lipophilic balance) solid-phase extraction (SPE) cartridges were used. The limits of detection (LOD) in distilled water and the blank surface water were in the range of 0.006 - 0.65 and 1.66 - 45.05 pg/mL, respectively. The limits of quantitation (LOQ) for the distilled water and the blank surface water were in the range of 0.02 - 2.17 and 5.52 - 150.15 pg/mL, respectively. The absolute recoveries for fortified water samples were between 62.1% and 125.4%. Intra-day precision and accuracy for the blank surface water were 2.9% - 24.1% (R.S.D.) and -16.3% - 16.3% (bias), respectively. In surface wastewater near rivers, chlortetracycline and acetylsalicylic acid were detected frequently in the range of 0.017 - 5.404 and 0.029 - 0.269 ng/mL, respectively. Surface water near rivers had higher levels than surface water of domestic treatment plants.

• Journal of Microbiology and Biotechnology
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• v.21 no.1
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• pp.100-108
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• 2011

A method for the rapid detection and quantification of Newcastle disease virus (NDV) produced in an animal cell culture-based production system was developed to enhance the speed of the NDV vaccine manufacturing process. A SYBR Green I-based real-time RT-PCR was designed with a conventional, inexpensive RT-PCR kit targeting the F gene of the NDV LaSota strain. The method developed in this study was validated for specificity, accuracy, precision, linearity, limit of detection (LOD), limit of quantification (LOQ), and robustness. The validation results satisfied the predetermined acceptance criteria. The validated method was used to quantify virus samples produced in an animal cell culture-based production system. The method was able to quantify the NDV samples from mid- or late-production phases, but not effective on samples from the early-production phase. For comparison with other quantifiable methods, immunoblotting, plaque assay, and tissue culture infectious dose 50 ($TCID_{50}$) assay were also performed with the NDV samples. The results demonstrated that the real-time RT-PCR method is suitable for the rapid quantification of virus particles produced in an animal cell-culture-based production system irrespective of viral infectivity.

• Bulletin of the Korean Chemical Society
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• v.33 no.2
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• pp.559-563
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• 2012

An analytical method for the simultaneous determination of veterinary medicines (amprolium and decoquinate) in cattle and chicken's muscle by HPLC/UV-vis was established. Samples were extracted by a HLB (Hydrophilic-Liphophilic Balance) cartridge with acetonitrile and methanol. Prior to HPLC injection, a mixture solvent (Water:MeOH, 1:1) was utilized as a reconstitution solvent. Chromatographic separation was achieved with a C18 column ($250{\times}4.6mm$, $5{\mu}m$) using gradient elution with 20 mM HFBA and MeOH:ACN (1:1.8). The calibration curves from the spiked blank matrix showed good linearity (above $r^2$=0.997) in the concentration range of $0.13-12.0mg\;kg^{-1}$. The relative recovery (accuracy) and limit of quantitation (LOQ) were in the range of 78.5-107.1% and $0.13-0.42mg\;kg^{-1}$, respectively. The developed method can be used to determine under the MRL (Maximum Residue Limits) levels of veterinary medicines in animal tissues.

• Korean Journal of Pharmacognosy
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• v.44 no.4
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• pp.350-361
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• 2013

Asarum sieboldii has been used for treatment of fever, pain, common cold, and chronic sinusitis in Korea. In this study, we performed quantification analysis of seven major constituents including aristolochic acid I, aristolochic acid II, ${\alpha}$-asarone, ${\beta}$-asarone, elemicin, methyl eugenol, and safrole in the 70% ethanol extract of Asarum sieboldii and its solvent fractions, n-hexane, ethylacetate, n-butanol, and water ones using a ultra-performance liquid chromatography-electrospray ionization-mass spectrometer(UPLC-ESI-MS) and gas chromatography-mass spectrometer(GC-MS). Regression equations of seven components were acquired with $r^2$ values >0.99. The values of limit of detection(LOD) and quantification(LOQ) were 0.1-3.9 ng/mL and 0.3-11.7 mg/mL, respectively. The amount of the seven compounds in Asarum sieboldii were not detected -143.66 mg/g. The established LC-MS/MS and GC-MS methods will be helpful to improve quality control of Asarum sieboldii.

• Korean Journal of Veterinary Service
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• v.43 no.3
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• pp.189-196
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• 2020

This study was conducted to analyze feasibility of monitoring of fluoroquinolnes residual through feather analysis in broilers. The calibration curve showed good linearity (r²≥0.99) within the concentration range of 1~100 ㎍/kg. The limit of detection (LOD) and limit of quantification (LOQ) were validated at ≤0.66 and ≤1.99 ㎍/kg in broiler feather, respectively. The recoveries in feather samples ranged from 94.6 to 114.4% (5.1-15.8% RSD) at the 5 to 20 ㎍/kg spiking levels. The proposed new analytical method proved to be suitable and effective for fluoroquinolnes determination. We also monitored fluoroquinolones residue in 36 samples (broiler that were slaughtered in Gyonggi-do) using this method. Among tested feather samples, enrofloxacin and ciprofloxacin were detected in all samples. In muscle samples, enrofloxacin was detected in 20 (55.6%) samples and ciprofloxacin was not detected.

• Bulletin of the Korean Chemical Society
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• v.34 no.9
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• pp.2787-2794
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• 2013

Cholesterol and cholesterol oxidation products (COPs) may accumulate in foods of animal origin during processing or storage. An effective and sensitive analytical method was developed by increasing the UV absorption of compounds through derivatization by attaching a chromophore to the functional groups of cholesterols (cholesterol, 20-hydroxycholesterol, 7-ketocholesterol, cholestane-$3{\beta}$-$5{\alpha}$-$6{\beta}$-triol, 25-hydroxycholesterol, and $5,6{\alpha}$-epoxycholesterol). The influences of the reaction time, volume of reaction solvent, amounts of derivatizing reagent, and extraction solvents were investigated, as they may influence the reaction and extraction yield. The derivatized COPs were analyzed simultaneously on a C18 column (2.1 mm i.d. ${\times}$ 100 mm length, $3.5{\mu}m$ particle size) using a gradient elution with water and acetonitrile. The derivatized COPs showed increased sensitivity and selectivity in HPLC/UV-Vis. The LOD and LOQ were in the concentration ranges of 0.018-0.55 mg/kg and 0.059-1.84 mg/kg from the powdered milk. And the accuracy and precision were 78.1-116.7% and 1.1-9.9%, respectively.