• Title/Summary/Keyword: 잔류용매

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Improvement of analytical method for pymetrozine in citrus fruits (감귤류 과일의 피메트로진 정량을 위한 분석법 개선)

  • Jeon, Jun-Ho;Chun, Su-Hyun;Kim, Min-Hyuk;Kim, Mi-Ok;Lee, Kwang-Won
    • Korean Journal of Food Science and Technology
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    • v.51 no.4
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    • pp.316-323
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    • 2019
  • It is difficult to analyze pymetrozine in citrus fruits using the hydromatrix method because of its low efficiency of purification and overlap of matrix and pymetrozine peaks. Liquid-liquid extraction can analyze pymetrozine in citrus fruits using dichloromethane. Since low pH interferes with the extraction of pymetrozine, the extracts of citrus fruits were maintained over pH 7.0 by adding borax buffer and 1 N NaOH in the improved method. According to the improved method, citrus fruits (such as lemon, lime, orange, tangerine, and grapefruit) were extracted and purified for HPLC-photo diode array analysis. The results of validation were as follows: $4.360{\mu}g/kg$ of limit of detection, $14.533{\mu}g/kg$ of limit of quantitation, and 0.007 mg/kg of method quantitative limit. Citrus fruits spiked with pymetrozine showed a recovery range from 71.8 to 83.7% and a coefficient of variation below 6%. Thus, the improved method can efficiently analyze pymetrozine in citrus fruits.

Optimization and Stabilization of Automated Synthesis Systems for Reduced 68Ga-PSMA-11 Synthesis Time (68Ga-PSMA-11 합성 시간 단축을 위한 자동합성장치의 최적화 및 안정성 연구)

  • Ji hoon KANG;Sang Min SHIN;Young Si PARK;Hea Ji KIM;Hwa Youn JANG
    • Korean Journal of Clinical Laboratory Science
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    • v.56 no.2
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    • pp.147-155
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    • 2024
  • Gallium-68-prostate-specific membrane antigen-11 (68Ga-PSMA-11) is a positron emission tomography radiopharmaceutical that labels a Glu-urea-Lys-based ligand with 68Ga, binding specifically to the PSMA. It is used widely for imaging recurrent prostate cancer and metastases. On the other hand, the preparation and quality control testing of 68Ga-PSMA-11 in medical institutions takes over 60 minutes, limiting the daily capacity of 68Ge/68Ga generators. While the generator provides 1,110 MBq (30 mCi) nominally, its activity decreases over time, and the labeling yield declines irregularly. Consequently, additional preparations are needed, increasing radiation exposure for medical technicians, prolonging patient wait times, and necessitating production schedule adjustments. This study aimed to reduce the 68Ga-PSMA-11 preparation time and optimize the automated synthesis system. By shortening the reaction time between 68Ga and the PSMA-11 precursor and adjusting the number of purification steps, a faster and more cost-effective method was tested while maintaining quality. The final synthesis time was reduced from 30 to 20 minutes, meeting the standards for the HEPES content, residual solvent EtOH content, and radiochemical purity. This optimized procedure minimizes radiation exposure for medical technicians, reduces patient wait times, and maintains consistent production schedules, making it suitable for clinical application.

Effect of Repetitive Transcranial Magnetic Stimulation in Drug Resistant Depressed Patients (치료 저항성 우울증 환자에서 반복적 경두개 자기자극후 국소뇌혈류 변화)

  • Chung, Yong-An;Yoo, Ie-Ryung;Kang, Bong-Joo;Chae, Jeong-Ho;Lee, Hye-Won;Moon, Hyun-Jin;Kim, Sung-Hoon;Sohn, Hyung-Sun;Chung, Soo-Kyo
    • Nuclear Medicine and Molecular Imaging
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    • v.41 no.1
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    • pp.9-15
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    • 2007
  • Purpose: Repetitive transcranial magnetic stimulation (rTMS) has recently been clinically applied in the treatment of drug resistant depressed patients. There are mixed findings about the efficacy of rTMS on depression. Furthermore, the influence of rTMS on the physiology of the brain is not clear. We prospectively evaluated changes of regional cerebral blood flow (rCBF) between pre- and post-rTMS treatment in patients with drug resistant depression. Materials and Methods: Twelve patients with drug-resistant depression (7 male, 5 female; age range: $19{\sim}52$ years; mean age: $29.3{\pm}9.3$ years) were given rTMS on right prefrontal lobe with low frequency (1 Hz) and on left prefrontal lobe with high frequency (20 Hz), with 20-minute-duration each day for 3 weeks. Tc-99m ECD brain perfusion SPECT was obtained before and after rTMS treatment. The changes of cerebral perfusion were analyzed using statistical parametric mapping (SPM; t=3.14, uncorrected p<0.01, voxel=100). Results: Following areas showed significant increase in rCBF after 3 weeks rTMS treatment: the cingulate gyrus, fusiform gyrus of right temporal lobe, precuneus, and left lateral globus pallidus. Significant decrement was noted in: the precental and middle frontal gyrus of right frontal lobe, and fusiform gyrus of left occipital lobe. Conclusion: Low-frequency rTMS on the right prefrontal cortex and high-frequency rTMS on the left prefrontal cortex for 3 weeks as an add-on regimen have increased and decreased rCBF in the specific brain regions in drug-resistant depressed patients. Further analyses correlating clinical characteristics and treatment paradigm with functional imaging data may be helpful in clarifying the pathophysiology of drug-resistant depressed patients.

Development and Validation of Analytical Method for Determination of Fungicide Spiroxamine Residue in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Spiroxamine의 시험법 개발 및 검증)

  • Park, Shin-Min;Do, Jung-Ah;Lim, Seung-Hee;Yoon, Ji-Hye;Pak, Won-Min;Shin, Hye-Sun;Kuk, Ju-Hee;Chung, Hyung-Wook
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.296-305
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    • 2018
  • Spiroxamine, one of fungicides, is used to control powdery mildew in various crops and black yellow sigatoka in bananas. The major strength of spiroxamine is to control powdery mildew in various crops and bananas yellow sigatoka in bananas. The compound has shown a high level of activity, good persistence and crop tolerance. Besides powdery mildew, good control of rust, net blotch and Rhynchosporium diseases been indicated in cereals, together with a complementary activity against Septoria diseases. In 2017, the maximum residue limit (MRL) of spiroxamine established in Korea. According to Ministry of ood and rug afety) regulations, spiroxamine residues defined only parent compound. Thus, a analytical method is needed to estimate the residue level of the parent compound. The objective of this study was to develop and validate analytical method for spiroxamine in representative agricultural commodities. Samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interfering substances. The analyte were quantified and confirmed liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive-ion mode using multiple reaction monitoring (MRM). Matrix matched calibration curves were linear over the calibration ranges ($0.0005{\sim}0.1{\mu}g/mL$) for the analyte in blank extract with coefficient of determination ($r^2$) > 0.99. For validation purposes, recovery studies will be carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries 70.6~104.6% with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges in the Codex guidelines (CAC/GL40, 2003) and MFDS guidelines. proposed analytical method be used as an official analytical method in the Republic of Korea.

Antimicrobial, Antioxidant, and Anticoagulation Activities of Salicornia europaea seeds (함초 씨의 항균, 항산화 및 항혈전 활성)

  • Kim, Mi-Sun;Kim, Deuk Hoi;Sohn, Ho-Yong
    • Microbiology and Biotechnology Letters
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    • v.44 no.4
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    • pp.452-460
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    • 2016
  • This study was designed to develop a functional pharma-food using Salicornia europaea (SE). Tiny seeds from the mature SE were collected, and their biological activities were evaluated. The extraction yield of the seed in hot water was found to be 29.6% and the hot water extract (HWE) contained 25.7 mg/g total polyphenol (TP) and 11.5 mg/g total flavonoid (TF), which are similar to those contained in leaf and stem of SE. Among the subsequent organic solvent fractions, the ethylacetate (EA) fraction exhibited the highest content of TP (158.3 mg/g), TF (136.2 mg/g), and total sugar (228.3 mg/g). The EA fraction exhibited broad-range antibacterial activities against gram-positive bacteria, and the butanol fraction exhibited growth inhibitory effect against only Staphylococcus epidermidis. An antioxidation activity assay of the HWE and its fractions showed the EA fraction to have the highest radical scavenging activity with $RC_{50}$ values of 57.0, 29.0, and $28.9{\mu}g/ml$ against DPPH anion, ABTS cation, and nitrite, respectively. The $RC_{50}$ values of vitamin C against DPPH anion, ABTS cation, and nitrite were 10.7, 4.0, and $18.0{\mu}g/ml$, respectively, indicating that the EA fraction of SE has potent antioxidant compounds. In an anticoagulation assay, the EA fraction exhibited a 15-fold extended thrombin time at 5 mg/ml and activated partial thromboplastin time at 7 mg/ml, which are comparable to the activities of aspirin. The HWE and its fractions had no hemolysis activities against human RBCs at up to 1 mg/ml. These results suggest that the EA fraction from SE has a great potential as a new antibacterial and anticoagulation agent.

Development of an Analytical Method for the Determination of Pyriofenone residue in Agricultural Products using HPLC-UVD (HPLC-UVD를 이용한 농산물 중 살균제 pyriofenone 분석법 확립)

  • Park, Hyejin;Kim, HeeJung;Do, Jung-Ah;Kwon, Ji-Eun;Yoon, Ji-Young;Lee, Ji-Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • 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.

Investigation on the Material and Migration Tests of Gas Impermeable Plastic Vacuum Packaging Materials for Food-Contact Use (식품용 합성수지제 공기차단성 포장재에서의 재질 및 용출시험량 조사)

  • Lee, Jung-Pyo;Lee, Youn-Kyu;Lee, Keun-Taik
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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    • v.14 no.1
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    • pp.35-42
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    • 2008
  • Twenty eight gas impermeable plastic films for food-contact application were collected in the domestic market and material and/or migration tests for overall migration, antioxidants, potassium permanganate consumption, heavy metal, and plasticizers were carried out. The average overall migration values for NY/PE or NY/LLDPE, PETP/PE, and PVDC packaging films obtained by using n-heptane as fatty food simulant were 7.6, 6.9 and 14.1 mg/L, respectively. These values were much lower than the limit values of 150 and 30 mg/L for polyethylene and polyvinylidene chloride prescribed in the Korea Food Code. In almost of the packaging materials tested, the antioxidants such as Irganox 1010, Irganox 1076 and Irgafos 168 were found. The migration test result showed that almost of all samples except PVDC film contained Irganox 1076 and Irgafos 168, while the maximum migration value of Irganox 1076 into n-heptane was found in the Ny/PE/LLDPE(15/25/50 ${\mu}m$) sample at the concentration of 216.9 ${\mu}g/g$. From the plastic packaging samples tested, plasticizers such as DEP, DPRP, DBP, DPP, BBP, DCHP, DEHP, DEHA and observed above the detection limit. Consumption amount of potassium permanganate was much lower than the limit value of 10 mg/L. In the material test for heavy metals, cadmium and lead were determined at the concentrations far below the limit value of 100 mg/kg. The migration test for cadmium and lead showed a lower value than the detection limit. Therefore, it can be concluded that the safety status of the plastic films tested met the requirement of limit values as prescribed for the material and migration tests of food packaging utensils, containers and packages of the Korea Food Code.

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Effect of starch extraction solutions on extraction and physicochemical property of Chinese yam (Dioscorea batatas) starch (마(Dioscorea batatas) 전분의 추출 및 물리화학적 특성에 대한 전분추출용액의 영향)

  • Lee, Hyunjeong;Seo, Dong-Ho;Kim, Hyun-Seok
    • Korean Journal of Food Science and Technology
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    • v.50 no.2
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    • pp.191-197
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    • 2018
  • This study investigated the influence of starch extraction (ST-EX) solutions on the extraction yield and characteristics of Chinese yam (CY) starches from domestic Dioscorea batatas. Ascorbic acid (VitC), $Na_2S_2O_3$, $NaHCO_3$, and $Na_2CO_3$ were used as ST-EX solutions (0.4%, w/v). The extracted CY starches were examined for ST-EX yield, chemical composition, size distribution, X-ray diffraction, solubility, swelling power, gelatinization, and pasting viscosity. The highest ST-EX yield was obtained from $NaHCO_3$, followed by VitC. Lower protein content, relative crystallinity, and gelatinization enthalpy were found in CY starches from alkaline ST-EX solutions ($NaHCO_3$ and $Na_2CO_3$). Size distribution and gelatinization temperature did not generally differ for CY starches from the different ST-EX solutions. Pasting viscosities increased in the order from $Na_2CO_3$ > $Na_2S_2O_3$ > $NaHCO_3$ > VitC ST-EX solutions. Thus, VitC may be most appropriate to extract CY starch from Dioscorea rhizomes, considering its ST-EX yield, total starch content, and variation in pasting viscosity.

Biological Control of Fusarium Head Blight on Wheat by Polyacetylenes Derived from Cirsium japonicum Roots (대계근에서 분리한 Polyacetylene계 화합물을 이용한 밀 이삭마름병 방제)

  • Kim, Ji-In;Kim, Kihyun;Park, Ae Ran;Choi, Gyung Ja;Park, Hae Woong;Kim, In Seon;Kim, Jin-Cheol
    • Research in Plant Disease
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    • v.22 no.3
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    • pp.145-151
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    • 2016
  • Chemical fungicides have reduced Fusarium head blight (FHB) severity. However, by the effects of fungicide residues, they can only be used up to 30 days before time of harvest. Therefore, the development of new biofungicides that are applicable until harvest is required. In order to select plant extracts having antifungal activity against Fusarium graminearum for the control of FHB, we investigated the inhibitory effects of 225 medicinal plant extracts on spore germination of F. graminearum. Of these plant extracts, the methanol extract of Cirsium japonicum (CJ) roots showed the strongest antifungal activity. Through solvent partitioning, repeated column chromatography, and spore germination bioassay, two chemicals were purified and then their chemical structures were identified as ciryneol C (CC) and 1-heptadecene-11,13-diyne-8,9,10-triol (HD-ol) which are polyacetylene substances. Two active compounds effectively inhibited the germination of F. graminearum macroconidia; HD-ol ($IC_{50}$ of $3.17{\mu}g/ml$) showed stronger spore germination inhibitory activity than that of CC ($IC_{50}$ of $28.14{\mu}g/ml$). In addition, the wettable powder type formulation of ethyl acetate extract of CJ roots suppressed the development of FHB in dose-dependent manner, with control values of 78.92% and 31.56% at 250- and 500-fold dilutions, respectively. Combining these findings suggest that the crude extract of CJ roots containing polyacetylene compounds could be used as botanical fungicide for the control of FHB.

Analysis of Methoxyfenozide and Bentazone in Plant with HPLC by pH-Adjusted Liquid-liquid Partition Cleanup (pH조절 분배추출에 의한 식물체 중 Methoxyfenozide와 Bentazone의 HPLC 분석)

  • Lo, Seog-Cho;Hwang, Cheol-Hwan;Yoo, Ki-Yong;Han, Seong-Soo
    • Korean Journal of Environmental Agriculture
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    • v.26 no.3
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    • pp.246-253
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    • 2007
  • This study was performed to enhance the cleanup efficiency of methoxyfenozide and bentazone by pH adjustment in the course of liquid-liquid partition and to develop an optimum analytical conditions using HPLC coupled with DAD for two matrices, brown rice and rice straw. Preparation procedure of brown rice sample was "extraction${\rightarrow}$coagulation${\rightarrow}$liquid-liquid partition$\rightarrow$-florisil C.C", and this procedure was samely applied to two compounds. In rice straw, preparation procedure of methoxyfenozide sample was "extraction$\rightarrow$-alkalization$\rightarrow$liquid-liquid extraction$\rightarrow$coagulation$\rightarrow$florisil C.C", and in the case of bentazone, "extraction$\rightarrow$alkalization$\rightarrow$liquid-liquid partition$\rightarrow$acidification$\rightarrow$liquid-liquid extraction$\rightarrow$florisil C.C". All these purified samples were redissolved in the mobile phases, acetonitile : 20 mM sodium acetate (75:25, v/v) for methoxyfenozide and acetonitrile : 75 mM sodium acetate, pH 6.0 (40:60, v/v) for bentazone. Recoveries of methoxyfenozide analysis in brown rice and rice straw were 83.5-97.4 and 86.4-97.3%, and detection limits were 0.02 and 0.04 mg/kg, respectively. Recoveries of bentazone in brown rice and rice straw were 86.8-101.9 and 88.3-94.5% and detection limits were 0.005 and 0.01 mg/kg, respectively. This methods seem to be usefully applied to the residue analysis of two compounds in the view of producing stable analytical condition and fair reproducibility.