• Korean Journal of Food Science and Technology
• /
• v.41 no.3
• /
• pp.326-333
• /
• 2009

Heterocyclic aromatic amines (HCAs) are mutagenic and carcinogenic substances that are formed during the heating of protein-rich foods. HCAs are generally found at low amounts in a complex matrix, which requires sophisticated analysis. In this study, HCAs were extracted from lyophilized fish and shellfish samples using solid-phase extraction (SPE) and determined by liquid chromatography-electrospray ionization/mass spectrometry (LC-ESI-MS). The HCA recoveries in the fish and shellfish ranged from 15.7 to 74.7% with standard deviations from 0.2 to 7.63%. And HCA concentrations ranged from 0.8 to 1,117.7 $ng/g^{-1}$ in cooked food samples. 1-methyl-9H-pyrido[3,4-b]indole (Harman), 9H-pyrido[3,4-b]indole (Norharman), and 2-amino-1-methyl-6-phenylimidazo[4,5-b]pyridine (PhIP) were the most abundant HCAs formed in the muscle of fried mackerel, at levels of 1,117.7, 926.6, and 133.7 ng/g, respectively. 3-amino-1-methyl-5H-pyrido[4,3-b]indole (Trp-P-2), 2-aminodipiryrido[1,2-a:3,2-d]imidazole(Glu-P-2), 2-amino-9H-pyrido[2,3-b]indole(A${\alpha}$C), 2-amino-3methyl-9H-pyrido [1,2-a:3,2-d]imidazole(MeA${\alpha}$C), 2-amino-3,4,7,8-tetramethylimidazo[4,5-f]quinoxaline (TriMeIQx), 2-amino-3,7,8-trimethylimidazo [4,5-f]quinoxaline(7,8-DiMeIQx), and 2-amino-3,8-dimethylimidazo[4,5-f]quinoxaline (MeIQx) were only detected by small quantities ranged from 1.5 to 98.6 ng/g. Overall, this study provides useful information on HCA levels in fish and shellfish products consumed in Korea.

• Journal of Food Hygiene and Safety
• /
• v.37 no.3
• /
• pp.136-142
• /
• 2022

The research aims to develop a rapid and easy analytical method for methoprene using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A simple, highly sensitive, and specific analytical method for the determination of methoprene in livestock products (beef, pork, chicken, milk, eggs, and fat) was developed. Methoprene was effectively extracted with 1% acetic acid in acetonitrile and acetone (1:1), followed by the addition of anhydrous magnesium sulfate (MgSO₄) and anhydrous sodium acetate. Subsequently, the lipids in the livestock sample were extracted by freezing them at -20℃. The extracts were cleaned using MgSO₄, primary secondary amine (PSA), and octadecyl (C₁₈), which were then centrifuged to separate the supernatant. Nitrogen gas was used to evaporate the supernatant, which was then dissolved in methanol. The matrix-matched calibration curves were constructed using 8 levels (1, 2.5, 5, 10, 25, 50, 100, 150 ng/mL) and the coefficient of determination (R²) was above 0.9964. Average recoveries spiked at three levels (0.01, 0.1, and 0.5 mg/kg), and ranged from 79.5-105.1%, with relative standard deviations (RSDs) smaller than 14.2%, as required by the Codex guideline (CODEX CAC/GL 40). This study could be useful for residue safety management in livestock products.

• Korean journal of applied entomology
• /
• v.27 no.2
• /
• pp.117-124
• /
• 1988

An Investigation of insect pests in rice stored was carried out in Jeonnam region of Korea. The total of 2 class, 7 orders 16 families and 25 species were recorded in Lepidoptera; 8, Coleoptera; 11, Orthoptera; 1, Thysanura 1, blattaria; 2, Hymenoptera; 1 and mites; 2 spe-cies. The important species among them were Sitotroga cerealella, Ephestia cautella, Paral-ipsa gularis, Poldia, in Lepidoptera, and Sitophilus orzae, Oryzaephilus surianmensis, Cryptolestes ferrugineus, Tribolium castaneum, Tenebroides mauritanicus, Attagenus japonicus, in Coleoptera and Blatella germanica, in Blattaria and Acarus siro Petrobia latens, in mites. The duration of maximum occurrence were the late June to mid July for Sitotroga cerealella, the mod July to early August for Oryzaephilus surianmensis the mid July to August for Tribolium castaneum, the early July to late July for Sitophilus orzae, the mid June to early July for Attagenus japonicus the mid June to late Spetember for Blatella germanica and the late April to late May for Acarus siro and Petrobia latens, respectively in investigation, Blatella germanica(Blattaria) which was no problem in stored rice insect till now was mainly distributed a coastal plain and period of occurrence was long amount of occurrence was great. Rice weevil has 4 generations under natural conditions and the peak of 1st perood time was ranged from middle of jun. to last decade of Jun., 2nd period was from the lats decade of Jul. to first decade of Aug., 3rd period was from middle of Sep. to late Sep., 4th period was middle of Oct. to early Nov.

• Korean Journal of Environmental Agriculture
• /
• v.36 no.1
• /
• pp.43-49
• /
• 2017

BACKGROUND: Greenhouse crops are one of agricultural products consumed largely in Korea. Cucumber is a typical example as main vegetables of greenhouse crops. Thus, pesticide residue analysis is an important requirement to guarantee pesticide safety of cucumber. This work was aim to investigate the residues of penthiopyrad and pyriofenone in cucumber after harvest. METHODS AND RESULTS: Cucumber was subjected to treat with penthiopyrad and pyriofenone at a level of recommended dose 0, 1, 2, 3, 5, 7 and 10 days before harvest under greenhouse conditions. The samples were extracted with organic solvent by using a homogenizer and purified on solid phase cartridge column followed by LC-MS/MS analysis. The recovery levels of penthiopyrad and pyriofenoneranged from approximately 81 to 93% with the method limit of 0.005 mg/kg and coefficient of variation less than 10%. Penthiopyrad and pyriofenone were detected at a level less than maximum residue limit in cucumber at 10 days before. The half-lives of penthiopyrad and pyriofenone were determined to 2.4 ~ 2.6 days. CONCLUSION: Penthiopyrad and pyriofenone are suggested to use in cucumber 10 days before harvest to reach their levels less than maximum residue limit.

• Journal of Food Hygiene and Safety
• /
• v.36 no.3
• /
• pp.228-238
• /
• 2021

The aim of this research was to develop a rapid and easy multi-residue method for determining dimethipin, omethoate, dimethipin, chlorfenvinphos and azinphos-methyl in agricultural products (hulled rice, potato, soybean, mandarin and green pepper). Samples were prepared using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and analyzed using gas chromatography-tandem mass spectrometry (GC-MS/MS). Residual pesticides were extracted with 1% acetic acid in acetonitrile followed by addition of anhydrous magnesium sulfate (MgSO₄) and anhydrous sodium acetate. The extracts were cleaned up using MgSO₄, primary secondary amine (PSA) and octadecyl (C₁₈). The linearity of the calibration curves, which waas excellent by matrix-matched standards, ranged from 0.005 mg/kg to 0.3 mg/kg and yielded the coefficients of determination (R²) ≥ 0.9934 for all analytes. Average recoveries spiked at three levels (0.01, 0.1, 0.5 mg/kg) and were in the range of 74.2-119.3%, while standard deviation values were less than 14.6%, which is below the Codex guideline (CODEX CAC/GL 40).

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

• Journal of the Korean Society of Food Science and Nutrition
• /
• v.46 no.4
• /
• pp.459-464
• /
• 2017

Biphenyl is used as an intermediate in the production of crop protection products, a solvent in pharmaceutical production, and as a component in the preservation of citrus fruits in many countries. Biphenyl is not authorized for use and also does not have standards or specifications as a food additive in Korea. National and imported food products are likely to contain biphenyl. Therefore, control and management of these products is required. In this study, a simple analytical method was developed and validated using HPLC to determine biphenyl in food. These methods are validated by assessing certain performance parameters: linearity, accuracy, precision, recovery, limit of detection (LOD), and limit of quantitation (LOQ). The calibration curve was obtained from 1.0 to $100.0{\mu}g/mL$ with satisfactory relative standard deviations (RSD) of 0.999 in the representative sample (orange). In the measurement of quality control (QC) samples, accuracy was in the range of 95.8~104.0% within normal values. The inter-day and inter-day precision values were less than 2.4% RSD in the measurement of QC samples. Recoveries of biphenyl from spiked orange samples ranged from 92.7 to 99.4% with RSD between 0.7 and 1.7% at levels of 10, 50, and $100{\mu}g/mL$. The LOD and LOQ were determined to be 0.04 and $0.13{\mu}g/mL$, respectively. These results show that the developed method is appropriate for biphenyl identification and can be used to examine the safety of citrus fruits and surface treatments containing biphenyl residues.

• Restorative Dentistry and Endodontics
• /
• v.32 no.3
• /
• pp.169-179
• /
• 2007

This study was to compare the microshear bond strength $({\mu}SBS)$ of light- and chemically cured composites to enamel coupled with four 2-step self-etch adhesives and also to evaluate the incompatibility between 2-step self-etch adhesives and chemically cured composite resin. Crown segments of extracted human molars were cut mesiodistally, and a 1 mm thickness of specimen was made. They were assigned to four groups by adhesives used: SE group (Clearfil SE Bond) AdheSE group (AdheSE), Tyrian group (Tyrian SPE/One-Step Plus), and Contax group (Contax) Each adhesive was applied to a cut enamel surface as per the manufacturer's instruction. Light-cured (Filtek Z250) or chemically cured composite (Luxacore Smartmix Dual) was bonded to the enamel of each specimen using a Tygon tube. After storage in distilled water for 24 hours, the bonded specimens were subjected to ${\mu}SBS$ testing with a crosshead speed of 1 mm/minute. The mean ${\mu}SBS$ (n=20 for each group) was statistically compared using two-way ANOVA, Tukey HSD, and t test at 95% level. Also the interface of enamel and composite was evaluated under FE-SEM. The results of this study were as follows ; 1. The ${\mu}SBS$ of the SE Bond group to the enamel was significantly higher than that of the AdheSE group, the Tyrian group, and the Contax group in both the light-cured and the chemically cured composite resin (p < 0.05). 2. There was not a significant difference among the hdheSE group, the Tyrian group, and the Contax group in both the light-cured and the chemically cured composite resin. 3. The ${\mu}SBS$ of the light-cured composite resin was significantly higher than that of the chemically cured composite resin when same adhesive was applied to the enamel (p < 0.05). 4. The interface of enamel and all 2-step self-etch adhesives showed close adaptation, and so the incompatibility of the chemically cured composite resin did not show.

• Journal of Food Hygiene and Safety
• /
• v.38 no.5
• /
• pp.361-372
• /
• 2023

Organotin pesticide is used as an acaricide in agriculture and may contaminate livestock products. This study aims to develop a rapid and straightforward analytical method for detecting organotin pesticides, specifically azocyclotin, cyhexatin, and fenbutatin oxide, in various livestock products, including beef, pork, chicken, egg, and milk, using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The extraction process involved the use of 1% acetic acid in a mixture of acetonitrile and ethyl acetate (1:1). This was followed by the addition of anhydrous magnesium sulfate (MgSO₄) and anhydrous sodium chloride. The extracts were subsequently purified using octadecyl (C₁₈) and primary secondary amine (PSA), after which the supernatant was evaporated. Organotin pesticide recovery ranged from 75.7 to 115.3%, with a coefficient of variation (CV) below 25.3%. The results meet the criteria range of the Codex guidelines (CODEX CAC/GL 40). The analytical method in this study will be invaluable for the analysis of organotin pesticides in livestock products.

• The Korean Journal of Nuclear Medicine Technology
• /
• v.14 no.2
• /
• pp.104-109
• /
• 2010

Purpose: $[^{18}F]$Fallypride plays an effective radiotracer for the study of dopamine $D_2/D_3$ receptor occupancy, neuropsychiatric disorders and aging in humans. This tracer has the potential for clinical use, but automated labeling efficiency showed low radiochemical yields about 5~20% with relatively long labelling time of fluorine-18. In present study, we describe an improved automatic synthesis of [$^{18}F$]Fallypride using different base concentration for routine clinical use. Materials and Methods: Fully automated synthetic process of [$^{18}F$]Fallypride was perform using the TracerLab $FX_{FN}$ synthesizer under various labeling conditions and tosyl-fallypride was used as a precursor. [$^{18}F$]Fluoride was extracted with various concentration of $K_{2.2.2.}/K_2CO_3$ from $^{18}O$-enriched water trapped on the ion exchange cartridge. After azeotropic drying, the labeling reaction proceeded in $CH_3CN$ at $100^{\circ}C$ for 10 or 30 min. The reaction mixture was purified by reverse phase HPLC and collected organic solution was exchanged by tc-18 Sep-Pak for the clinically available solution. Results: The optimal labeling condition of [$^{18}F$]Fallypride in the automatic production was that 2 mg of tosyl-fallypride in acetonitrile (1 mL) was incubated at $100^{\circ}C$ for 10 min with $K_{2.2.2.}/K_2CO_3$ (11/0.8 mg). [$^{18}F$]Fallypride was obtained with high radiochemical yield about $66{\pm}1.4%$ (decay-corrected, n=28) within $51{\pm}1.2$ min including HPLC purification and solid-phase purification for the final formulation. Conclusion: [$^{18}F$]Fallypride was prepared with a significantly improved radiochemical yield with high specific activity and shorten synthetic time. In addition, this automated procedure provides the high reproducibility with no synthesis failures (n=28).