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Development and Validation of Analytical Methods for Picoxystrobin Determination in Agricultural Products by GC-ECD and GC-MS

  • Do, Jung-Ah;Lee, Min-Hye;Park, Hyejin;Kang, Il-Hyun;Kwon, Kisung;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.27 no.4
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    • pp.332-338
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    • 2012
  • A simple and sensitive analytical method was developed using gas chromatography with electron capture detector (GC-ECD) and gas chromatography-mass spectrometry (GC-MS) for determination of Picoxystrobin in agricultural products (apple, hulled rice, mushroom, pepper, soybean, and mandarin). Picoxystrobin residues were extracted with acetonitrile, partitioned with saline water, and then they were cleaned up on a florisil solid-phase extraction (SPE) cartridge to obtain an extract suitable for analysis by GC-ECD and GC-MS. The method was validated using 6 agricultural product samples spiked with Picoxystrobin at different concentration levels (0.02, 0.05 and 0.5 mg/L). Average recoveries of Picoxystrobin (using each concentration three replicates) ranged 64.0~98.3% with relative standard deviations less than 10%, calibration solutions concentration in the range 0.1~5 mg/L, and limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.02 mg/L, respectively. The result showed that the developed analytical method is suitable for Picoxystrobin determination in agricultural products.

Development and Validation of an Analytical Method for Tridemorph Determination in Tea Samples by Liquid Chromatograph-Electrospray Ionization-Tandem Mass Spectrometry

  • Do, Jung-Ah;Park, Hyejin;Kwon, Ji-Eun;Cho, Yoon-Jae;Chang, Moon-Ik;Oh, Jae-Ho;Hwang, In-Gyun
    • Journal of Food Hygiene and Safety
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    • v.29 no.4
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    • pp.292-298
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    • 2014
  • Tridemorph is a systemic morpholine fungicide for crops. The objective of this study was to develop reliable and sensitive analytical method for determination of tridemorph residues in tea samples for ensuring the food safety. Tridemorph residues in samples were extracted with acetonitrile after hydration, partitioned with saline water, and then purified using an aminopropyl ($NH_2$) SPE cartridge. The purified samples were detected and quantified using LC-ESI-MS/MS. The linear detection limits for tridemorph ranged from 0.02 to $1.0mgL^{-1}$ with a correlation coefficient of 0.9999. The method was validated using tea samples spiked with tridemorph at different concentration levels (0.02 and $0.05{\mu}gmL^{-1}$). The average recovery ranged between 75.0 and 84.7% with relative standard deviations less than 10%. The LOD and LOQ were 0.01 and $0.02mgL^{-1}$, respectively. The developed method was applied successfully to the identification of tridemorph in real tea samples obtained from different sources, and tridemorph was not detected in any of the samples. The results show that the developed analytical method is accurate and suitable for tridemorph determination in tea samples.

Comparison of Optimal Storage Temperature and Collection Reagents for Living Bacterial Cells in Swab Samples (면봉시료에서 세균의 보존을 위한 최적 보관 온도와 채취 시약의 비교)

  • Lee, Yeong Ju;You, Hee Sang;Lee, Song Hee;Lee, So Lip;Lee, Han;Sung, Ho Joong;Kang, Hee Gyoo;Hyun, Sung Hee
    • Korean Journal of Clinical Laboratory Science
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    • v.53 no.4
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    • pp.326-332
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    • 2021
  • Swabs are useful and common sampling tools in various research fields, such as medicine, ecology, biotechnology, forensic medicine, and pollutant monitoring systems. Collection reagents are one of the essential components in sampling. It is important to develop a sample collection kit and designate an appropriate storage temperature because samples need to be stored for a long time. The purpose of this study was to identify the effects of three collection reagents and three storage temperatures on the recovery of living bacteria without media. We selected Escherichia coli and Staphylococcus aureus as representative environmental bacteria. Distilled water (DW), phosphate buffered saline (PBS), and Tris-EDTA (TE) buffer were used as collection reagents and stored at 22℃, 4℃, and -70℃ after sampling. The results of using each collection reagent and storage temperature on the bacteria were compared using relative light units (RLU) and the number of colony forming units (CFU). When using -70℃ storage temperature and the TE buffer, the number of living bacteria and the RLU values remained constant. It is therefore recommended that the sample be stored at -70℃ immediately after collection and a TE buffer solution be used as the collection reagent.

Development of Individual Residue Analysis Method for Cyanazine in Agricultural Commodities as an Unregistered Herbicide in Korea (국내 미등록 제초제 cyanazine의 농산물 중 개별 잔류분석법 개발)

  • Choung, Myoung-Gun;Im, Moo-Hyeog
    • Journal of the Korean Society of International Agriculture
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    • v.30 no.4
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    • pp.339-346
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    • 2018
  • Cyanazine is a member of the triazine family of herbicides. Cyanazine is used as a pre- and post-emergence herbicide for the control of annual grasses and broadleaf weeds. This experiment was conducted to establish a determination method for cyanazine, as domestic unregistered pesticide, residue in major agricultural commodities using HPLC-DAD/MS. Cyanazine was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and partitioned to dichloromethane for remove polar extractive in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized florisil column chromatography. On a $C_{18}$ column in HPLC, cyanazine was successfully separated from co-extractives of sample, and sensitively quantitated by diode array detection at 220 nm. Accuracy and precision of the proposed method was validated by the recovery experiment on every major agricultural commodity samples fortified with cyanazine at 3 concentration levels per agricultural commodity in each triplication. Mean recoveries were ranged from 83.6 to 93.3% in five major representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation(LOQ) of cyanazine was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring(SIM) technique was also provided to clearly identify the suspected residue.

Changes in CT Number and Noise Level according to Pitch in Spiral Image Acquisition (나선형영상획득에서 Pitch에 따른 CT 감약계수와 잡음의 변화)

  • Kang, SungJin
    • Journal of the Korean Society of Radiology
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    • v.14 no.7
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    • pp.981-989
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    • 2020
  • In this study, a self-made customized phantom was used to quantitatively measure the change in CT number and noise according to the change of pitch. In order to acquire an image using the phantom, the inside of the phantom was filled with sterile distilled water. Inside the glass tube, a solution obtained by diluting the ratio of normal saline and contrast medium to 100%(NS), 400:1, 200:1, 100:1, 50:1, respectively, was placed and imaged. At this time, the pitch was divided into steps of 0, 0.35, 0.7, 1.05, and 1.4 for each dilution ratio of the solution and imaged, respectively. One-way ANOVA analysis were performed to verify whether the mean of the CT number and noise values measured in all ROIs by dilution ratio showed a significant difference according to the change in pitch. As a result of the experiment, there was no statistically significant difference in the change of the CT number according to the change in the pitch for each dilution ratio, but the noise value tended to increase with the increase of the pitch, and showed a statistically significant difference. In the spiral image acquisition of CT, noise can be changed to a significant level depending on the pitch. Therefore, it will be necessary to set the quality evaluation items and criteria for CT images using the spiral image acquisition method.

Changes in sedimentary structure and elemental composition in the Nakdong Estuary, Korea (낙동강 하구역 퇴적구조 및 원소조성 변화에 관한 연구)

  • Kim, Yunji;Kang, Jeongwon;Park, Seonyoung
    • Journal of Wetlands Research
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    • v.23 no.3
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    • pp.213-223
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    • 2021
  • To understand the sedimentary environment of Scirpus planiculmis habitat (Myeongji and Eulsuk tidal flats) in the Nakdong Estuary, this study analyzed the statistical parameters (sorting, skewness, and kurtosis) of grain size data and the major (Al, Fe, Mn, Mg, Ca, Na, K, Ti, and P), minor (Li, Sc, V, Cr, Co, Ni, Cu, Zn, Sr, Zr, Cs, Pb, Th, and U), and rare earth elements (REEs) in sediment cores. For Myeongji, the sediment structure of the upper part of the cores was poorly sorted, more finely skewed, and more leptokurtic due to construction of the West gate. By contrast, the Eulsuk cores all differed due to the contrasting floodgate operation patterns of the West and East gates. The linear discriminate function (LDF) results corresponded to the statistical parameters for grain size. At the Eulsuk tidal flat (sites ES05 and ES11), elemental distributions were representative of Al-, Fe- and Ca-associated profiles, in which the elements are largely controlled by the accumulation of their host minerals (such as Na- and K-aluminosilicate and ferromagnesium silicate) and heavy detrital minerals at the sites. Detrital minerals including the aluminosilicates are major factors in the elemental compositions at ES05, diluting the REE contents. However, clay minerals and Fe-oxyhydroxides, as well as REE-enriched heavy minerals, appeared to be controlling factors of the elemental composition at ES11. Therefore, the mineral fractionation process is important in determining the elemental composition during sedimentation, which reflects the depositional condition of riverine-saline water mixing at both sites.

Zinc Deficiency Elevates Fecal Protein, But Not Electrolyte and Short-Chain Fatty Acid, Levels in Enterotoxigenic Escherichia coli-Induced Diarrhea in Rats

  • David, Ebuka E.;Yameen, Muhammad A.;Igwenyi, Ikechuku O.;David, Chidinma N.;Nwobodo, Valentine;Ismail, Akindele K.
    • Pediatric Gastroenterology, Hepatology & Nutrition
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    • v.25 no.1
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    • pp.79-86
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    • 2022
  • Purpose: To determine the effect of zinc deficiency on fecal protein, electrolyte, and short-chain fatty acid levels in both heat-stable (ST) and heat-labile (LT) enterotoxigenic Escherichia coli (ETEC)-induced diarrhea in rats. Methods: Albino rats, weighing 100 to 150 g, were divided into 2 groups, with 15 animals each: non-zinc and zinc-deficient. These two groups were sub-divided into three sub-groups with five rats each: control (saline); LT-ETEC; and ST-ETEC. Sodium phytate (30 mmol/L) was added to the animals' water to induce zinc deficiency, while diarrhea was induced using 5×109 ETEC cells/mL. Fecal protein levels were estimated using the Bradford method, while sodium and potassium levels were determined using atomic absorption spectrophotometry. Short-chain fatty acids were measured using gas chromatography-mass spectrometry. Results: Among the non-zinc and zinc-deficient groups, there were significant increases (p=0.04), (p=0.03) in fecal protein concentrations (mg/mL) in the LT-ETEC- (4.50±0.33), (6.50±0.26) and ST-ETEC- (3.85±0.19), (5.98±0.32) induced groups compared to the control groups (2.60±0.52), (3.50±0.11) respectively. Fecal sodium and potassium levels (mg/L) were significantly (p=0.029) increased in non-zinc-deficient rats induced with LT-ETEC (9.35±0.95, 1.05±0.48), and ST-ETEC (9.96±1.02, 1.21±0.45) compared with the control group (8.07±0.44, 0.47±0.17) but the increase were not statistically significant (p=0.059) in the zinc deficient rat groups. Fecal acetate and propionate levels (mg/g) significantly (p=0.032) increased when induced with LT-ETEC and ST-ETEC in non-zinc and zinc-deficient groups compared with the control groups. Conclusion: Zinc deficiency among rats with ETEC-induced diarrhea elevated fecal protein loss but may not have an effect on fecal sodium, potassium and short-chain fatty acid levels.

Effects of Sunbanghwalmyung-Eum Gamibang on MIA-Induced Osteoarthritis in Rats (흰쥐에서 MIA로 유발된 골관절염에 선방활명음 가미방이 미치는 영향)

  • You Bin, Shin;Han Byeol, Park;Jae Su, Kim;Hyun Jong, Lee;Sung Chul, Lim;Yun Kyu, Lee
    • Korean Journal of Acupuncture
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    • v.39 no.4
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    • pp.152-171
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    • 2022
  • Objectives : This study was designed to investigate the effects of Sunbanghwalmyung-eum gamibang on Monosodium iodoacetate-induced osteoarthritis rats. Methods : Forty Sprague-Dawley (SD) rats were divided into 5 groups of 8 rats each. Osteoarthritis (OA) was induced by injecting MIA (2 mg/50 µl) into the joint cavity of the left knee of SD rats belonging to the experimental group, and normal saline was injected into the joint cavity of the left knee instead of MIA in the normal group. To the normal group and the controlled group (OA group), 2 ml of distilled water was orally administered. To the positive control group (Indomethacin group), indomethacin 2 ml at a concentration of 2 mg/kg, to the low concentration group of SHG (Low group), 2 ml of SHG at a concentration of 2 mg/kg, and to the high concentration group of SHG (High group), 2 ml of SHG at a concentration of 4 mg/kg ml was orally administered. The drug was administered for a total of 4 weeks, and histological changes were analyzed by Hematoxylin-Eosin staining and Safranin-O staining. In addition, inflammatory cytokines such as TNF-α, IL-1β, and IL-6, and MMP-13, TIMP-1, and GAGs were immunohistochemically analyzed. Finally, hematological examination, blood biochemical examination, and liver and kidney biopsy were performed. Results : SHG groups (Low and High) inhibited the matrix destruction and damage of the knee joint cartilage in SD rat model, and significantly prevented the reduction in cartilage thickness. In SHG groups, the expressions of TNF-α, IL-1β, IL-6 and MMP-13 were significantly decreased, and the expressions of TIMP-1, GAGs were significantly increased compared with OA group. The safety indicators had no significant differences among five groups. Conclusions : These results show that SHG has cartilage protection capacity, anti-inflammatory effect.

Effect of New Herbal Mixture, HT008 on Arthritis Rat Model (한약복합물 HT008이 흰쥐 관절염 모델에 미치는 효과)

  • Lim, Dong-Wook;Kim, Mi-Yeon;Song, Mi-Kyung;Kim, Ji-Young;Lee, Dong-Hun;Park, Ju-Yeon;Bu, Young-Min;Kim, Ho-Cheol
    • The Korea Journal of Herbology
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    • v.24 no.4
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    • pp.197-204
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    • 2009
  • Objectives : This study was conducted to investigate the effect of HT008, a multi-herbal mixture consisting of 3 herbs, Eleutherococcus senticosus, Angelica sinensis, and Scutellaria baicaleinsis on arthritic model in rats. Methods : The anti-inflammatory and analgesic activities were observed by utilizing the following models: carrageenan-induced edema of the hind paw of rats, acetic acid-induced writhing response in mice. The perimeter of the paw was measured before injection and then at 1, 2, 4, 6 h after injection of 1% $\lambda$-carrageenan. The HT008 at five dose levels (10, 30, 100, and 300 mg/kg) and distilled water given 30 min to treatment groups and control group, before $\lambda$-carrageenan injection. In the writhing test, the mice received 0.7% acetic acid solution in normal saline injected intraperitoneally at a dose of 10 ml/kg. The number of writhes was counted staring 10 min after injection. Results : HT008 at four dose levels (30, 100, and 300 mg/kg) significantly decreased the carrageenan-induced rat paw edema perimeter. E. senticosus and S. baicaleinsis extracts reduced acetic acid-induced writhing response in mice. Also A. sinensis extracts significantly decreased the carrageenan-induced rat paw edema perimeter. Conclusions : These results show that HT008, a multi-herbal mixture has both anti-inflammatory activity and analgesic effects in vivo arthritic model, and suggest that HT008 could be a good therapy to treat human osteoarthritis.

Efficacy of Commercial Sanitizers for the Inactivation of Listeria monocytogenes on the Processing Equipment for Enoki Mushrooms (팽이버섯 재배 현장에서 Listeria monocytogenes의 성장을 억제하기 위한 살균 처리 기술 개발)

  • Kyung Min Park;Su-Bin Lee;Do-Young Jung;Song-Yi Choi;Injun Hwang;Se-Ri Kim
    • Journal of Food Hygiene and Safety
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    • v.38 no.6
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    • pp.508-516
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    • 2023
  • The consumption of enoki mushrooms has been associated with cases of listeriosis produced by Listeria monocytogenes, highlighting the significance of sanitizing food-contact surface, such as the velcro used in welding processing of enoki mushrooms, to ensure microbial safety. We investigated the inhibitory activity of nine chemical disinfectants at regular concentrations against L. monocytogenes isolated from a mushroom farm environment. The bacterial suspension was prepared in phosphate buffered saline and mushroom extract broth and inoculated onto the velcro surface. After inoculation, most disinfectants reduced the initial 8 log CFU/coupon concentration by less than 2 log CFU/coupon during a 5-min treatment. Slightly acidic hypochlorous water showed a reduction of approximately 4 log CFU/coupon when tested for more than 30 min at the maximum allowable concentration of 200 mg/L. Sodium hypochlorite solution showed a reduction of approximately 5 log CFU/coupon when used at 100 mg/L for 60 min. Peracetic acid, at the maximum allowable concentration of 300 mg/L, showed the most effective reduction of 5 log CFU/coupon or more when the surface was treated with 37.5 mg/L for 30 min. These results indicate that peracetic acid can be used as the disinfectant strategy to control cross-contamination of L. monocytogenes on the velcro surface of plastic wrappers used in the welding processing of enoki mushrooms.