• The Korean Journal of Pesticide Science
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• v.18 no.2
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• pp.79-87
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• 2014

Pyriofenone is an aryl phenyl ketone fungicide that is newly registered in Korea in 2013 to control powdery mildew on food. The objective of this study was to develop reliable and sensitive analytical method for determination of pyriofenone residue in agricultural products for ensuring the food safety. The pyriofenone residues in all samples(Korean melon, pepper, potato, mandarin, soybean, and hulled rice) were extracted with acetonitrile, partitioned with dichloromethane, and then purified with a silica cartridge. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. The linear range of pyriofenone was 0.05~5 mg/kg with the correlation coefficient ($r^2$) > 0.999. Average recoveries of pyriofenone ranged from 72.8% to 99.5% at the spiked level of 0.05 and 0.5 mg/kg, while the relative standard deviation was 2.3%~6.4%. In addition, the limit of detection and limit of quantification were 0.01 and 0.05 mg/kg, respectively. The results revealed that the developed and validated analytical method was suitable for pyriofenone determination in agricultural products.

• Journal of Veterinary Clinics
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• v.24 no.3
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• pp.308-311
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• 2007

A study on the oral bioavailability and pharmacokinetics of an anticoccidal agent, toltrazuril, was conducted in broilers following a single oral doses of 10 mg/kg body weight (BW) or 40 mg/kg BW. The concentrations of toltrazuril in plasma were determined by a high-performance liquid chromatography/mass spectrometry. Plasma concentration-time data after single oral administration were analyzed by a non-compartmental analysis. Toltrazuril was very well-absorbed through the gastrointestinal tract with $C_{max}$ of $18.04{\pm}5.80{\mu}g/mL$ and $47.15{\pm}9.40{\mu]g/mL$ at $4.33{\pm}1.51h$ and $3.67{\pm}1.15h$ after oral dose of 10 mg/kg and 40 mg/kg in broilers, respectively. A comparison between 10 mg/kg and 40 mg/kg dose groups showed that $t_{max}$ were similar while $C_{max}$ and area under curve (AUC) increased with increasing dose.

• Journal of Food Hygiene and Safety
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• v.32 no.5
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• pp.381-388
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• 2017

In this study, we investigated the levels of natural preservatives of benzoic acid, sorbic acid, and propionic acid in spices. The quantitative analysis was performed using high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) for benzoic acid and sorbic acid and gas chromatography-mass spectrometry (GC-MS) for propionic acid. The sample was extracted with ethanol using sonication, then centrifuged and evaporated to dryness and redissolved to 1 mL with ethanol to use for the instrumental analysis. The analytical method was validated based on linearity, recovery, limit of detection (LOD), and limit of quantification (LOQ). This method was suitable to determine low amounts of naturally occurring preservatives (benzoic acid, sorbic acid, and propionic acid) in various spices. Benzoic acid, sorbic acid, and propionic acid were found in 165 samples, 88 samples, and 398 samples, respectively from the total of 493 samples. The concentration of benzoic acid, sorbic acid, and propionic acid were ranged at ND-391.99 mg/L, ND-57.70 mg/L, and ND-188.21 mg/L in spices, respectively. The highest mean levels of benzoic acid, sorbic acid, and propionic acid were found in cinnamon (167.15 mg/L), basil leaves (22.79 mg/L), and white pepper (51.48 mg/L), respectively. The results in this study provide ranges of concentration regarding naturally occurring benzoic acid, sorbic acid, and propionic acid in spices. Moreover, the results may use to the case of consumer complaint or trade friction due to the inspection services of standard criteria for the preservatives of spices.

• Journal of Veterinary Clinics
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• v.29 no.3
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• pp.233-236
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• 2012

Cefquinome, a fourth generation cephalosporin, has been solely used for veterinary medicine and has a broad antibacterial spectrum against gram-negatives and gram-positives being very stable to ${\beta}$-lactamases. This study was conducted to evaluate the bioequivalence of two cefquinome 2.5% products in piglets. Plasma cefquinome concentrations were analyzed by liquid chromatography-mass spectrometry (LC/MS). Mean maximum concentration ($C_{max}$) of test product ($Cequus^{(R)}$) and reference product ($Cobactan^{(R)}$) were $4.34{\pm}0.58$ and $4.22{\pm}0.47{\mu}g/mL$, and mean area under the concentration time curve ($AUC_{0{\rightarrow}{\infty}}$) values were $10.43{\pm}1.96$ and $10.25{\pm}2.98{\mu}g{\cdot}h/mL$, respectively. The 90% confidence intervals for the ratio of $C_{max}$ (0.941-1.115), and $AUC_{0{\rightarrow}{\infty}}$ (0.927-1.172) values for the test and reference products were within the acceptable bioequivalence limit of 0.80-1.25. It is concluded that two commercial cefquinome injectable solutions are bioequivalent in their extent of drug absorption in piglets.

• Journal of Veterinary Clinics
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• v.23 no.2
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• pp.114-118
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• 2006

A study on bioavailability and pharmacokinetics of florfenicol was conducted in broilers following a single intravenous (i.v.) and oral (p.o.) doses of 20 mg/kg body weight (b.w.). Florfenicol concentrations in plasma were determined by a high-performance liquid chromatography/mass spectrometry. Plasma concentration-time data after i.v. administration were analyzed by a non-compartmental analysis. Following i.v. injection, the total body clearance was $0.74{\pm}0.25L/kg/h$ and the volume of distribution at steady-state was $1.16{\pm}0.19L/kg$. Florfenicol was rapidly distributed and eliminated following i.v. injection with $1.15{\pm}1.06h$ of elimination half-life. After oral administration, the calculated $C_{max}$ values ($8.18{\pm}0.97{\mu}g/mL$) were reached at $1.33{\pm}0.29h$ in broilers. The elimination half-life of florfenicol was $1.31{\pm}0.27h$ and the absolute bioavailability (F) was 75.46% after oral administration of florfenicol. Florfenicol amine, a major metabolite of florfenicol, was detected in all broilers after i.v. and p.o. administration of florfenicol. The observed $C_{max}$ values of florfenicol amine ($3.96{\pm}2.60\;and\;2.22{\pm}1.71{\mu}g/mL$) were reached at $0.16{\pm}0.19\;and\;1.61{\pm}1.02h$ after i.v. and p.o. administration of florfenicol, respectively. Florfenicol amine was eliminated with $1.88{\pm}0.39\;and\;2.64{\pm}1.39h$ of the elimination half-life after i.v. and p.o. administration of florfenicol, respectively.

• Korean Journal of Environmental Agriculture
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• v.32 no.1
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• pp.70-77
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• 2013

BACKGROUND: Nitroxoline is an antibiotic agent. It is used for the treatment of the second bacterial infection by the colibacillosis, salmonellosis and viral disease of the poultry. When the nitroxoline is indiscreetly used, the problem about the abuse of the antibiotics can occur. Therefore, this study presented the residue analytical method of nitroxoline in food for the safety management of animal farming products. METHODS AND RESULTS: A simple, sensitive and specific method for nitroxoline in chicken muscle by high performance liquid chromatograph with PDA was developed. Sample extraction with acetonitrile, purification with SPE cartridge (MCX) were applied, then quantitation by HPLC with C18 column under the gradient condition with 0.1 % tetrabutylammonium hydroxide-phosphoric acid and methanol was performed. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.999, analysed from 0.02 to 0.5 mg/L concentration. Limit of quantitation in chicken muscle showed 0.02 mg/kg, and average recoveries ranged from 72.9 to 88.1 % in chicken muscle. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 12 % in 0.02 and 0.04 mg/kg. CONCLUSION(S): Newly developed method for nitroxoline in chicken muscle was applicable to food inspection with the acceptable level of sensitivity, repeatability and reproducibility.

• Korean Journal of Food Science and Technology
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• v.45 no.6
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• pp.693-699
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• 2013

A simple, sensitive, and specific method for quantifying the nicotine content of synthetic favoring substances (SFS) was developed using high performance liquid chromatography (HPLC) with a photo-diode array detector (PDA). Nicotine was extracted from SFS samples by using an acid-base liquid-liquid extraction method with dichloromethane and distilled water. The nicotine content was quantified by HPLC/PDA (261.9 nm) with a $C_{18}$ column under a gradient of 10% acetonitrile with 20 mM ammonium formate (ammonia solution adjusted to pH 8.7) to 100% acetonitrile. The calibration curve, analyzed from concentration standards between 0.1 to 2 mg/L, presented linearity with a correlation coefficient ($r^2$)>0.9999. The limit of quantitation (LOQ) of nicotine in SFS was 0.4 mg/kg, and the average recoveries ranged from 76.4% to 96.3%. The repeatability of measurements, expressed as the coefficient of variation (CV%), ranged from 1.74 to 5.12%. This newly developed method for nicotine quantification in SFS can be considered an analytical method with an acceptable level of sensitivity and repeatability.

• Journal of Food Hygiene and Safety
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• v.33 no.2
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• pp.124-130
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• 2018

The Ministry of Food and Drug Safety (MFDS) is amending its test methods for the use of health functional foods (dietary food supplement), in order to establish regulatory standards and specifications in Korea. In this regard, we continue to pursue and perform our research on the analytical method development for the items being researched and reviewed. In this study, we have developed a sensitive and selective test method that could simultaneously separate and determinate six major bioactive flavonolignans in silymarin, which are based on the use of a liquid chromatographic-tandem mass spectrometry (LC-MS/MS). The standard calibration curves presented a linearity effect with the correlation coefficient ($r^2$) > 0.999. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of $0.3{\sim}9.0{\mu}g/L$ and $0.8{\sim}27.3{\mu}g/L$, respectively. The recovery results ranged between 96.2~98.6% at 3 different concentration levels, and its relative standard deviations (RSDs) were less than 5% as noted in this study. The proposed analytical method was characterized with a noted high resolution of the individual silymarin constituents, and the assay was fully validated as well. Our research can provide a significant scientific evidence that can be useful to amend the silymarin test method for the Health Functional Food Code.