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Determination and Validation of an Analytical Method for Spiropidion and Its Metabolite Spiropidion-enol (SYN547305) in Agricultural Products with LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Spiropidion 및 대사산물 Spiropidion-enol (SYN547305) 시험법 개발 및 검증)

  • Gu, Sun Young;Lee, Su Jung;Shin, Hye-Sun;Kang, Sung Eun;Chung, Yun Mi;Lee, Jung Mi;Jung, Yong-hyun;Moon, Guiim
    • Korean Journal of Environmental Agriculture
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    • v.41 no.2
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    • pp.82-94
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    • 2022
  • BACKGROUND: Spiropidion and its metabolite are tetramic acid insecticide and require the establishment of an official analysis method for the safety management because they are newly registered in Korea. Therefore, this study was to determine the analysis method of residual spiropidion and its metabolite for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods (original, AOAC, and EN method) were applied to optimize the extraction method, and the EN method was finally selected by comparing the recovery test and matrix effect results. Various adsorbent agents were applied to establish the clean up method. As a result, the recovery of spiropidion was reduced when using the dispersive-SPE method with MgSO4, primary secondary amine (PSA), graphitized carbon black (GCB) and octadecyl (C18) in soybean. Color interference was minimized by selecting the case including GCB and C18 in addition to MgSO4. This method was established as the final analysis method. LC-MS/MS was used for the analysis by considering the selectivity and sensitivity of the target pesticide and the analysis was performed in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 79.4-108.4%, with relative standard deviation and coefficient of variation were less than 7.2% and 14.4%, respectively. CONCLUSION(S): Spiropidion and its metabolite could be analyzed with a modified QuEChERS method, and the established method would be widely available to ensure the safety of residual insecticides in Korea.

Periprosthetic Fracture around Tumor Prosthesis, Comparison of Results with or without Cortical Strut Onlay Allograft (종양인공관절 주위 골절의 피질골 지주 중첩 동종골 이식술 유무에 따른 결과 비교)

  • Kim, Yongsung;Cho, Wan Hyeong;Song, Won Seok;Lee, Kyupyung;Jeon, Dae-Geun
    • Journal of the Korean Orthopaedic Association
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    • v.56 no.1
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    • pp.42-50
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    • 2021
  • Purpose: Periprosthetic fractures of a tumor prosthesis are rare but have difficulties in achieving sound fixation because of the poor bone quality, which increases the risk of loosening or re-fracture, even after bone union. A cortical strut onlay allograft was adopted for peri-prosthetic fractures after hip arthroplasty into the periprosthetic fracture of a tumor prosthesis, assuming that it would assist in firm fixation, shorten the time to union, and increase the bone stock, thereby, lower the chance of loosening and re-fracture. Materials and Methods: This study reviewed 27 patients (30 cases) of periprosthetic fracture of tumor prosthesis. Sixteen cases (allograft group) had augmentation with an onlay allograft, while 14 cases (conventional group) had internal fixation or conservative treatment. The following were assessed; mode of periprosthetic fracture, difference in the time to union between a strut cortical onlay allograft and without it, and survival of prosthesis, complication, and functional outcome between the two groups. Results: According to the unified classification system (UCS), 21 cases were type B (70.0%; B1, 14; B2, 1; B3, 6) and 9 cases were type C. The five-, 10-year survival of the 30 reconstructions by Kaplan-Meier plot was 84.5%±4.18% and 42.2%±7.83%, respectively. The average time to bone union of the entire cohort was 5.1 months (range, 2.0-11.2 months). The allograft group (3.5 months) showed a shorter period for union than the conventional group (7.2 months) (p<0.0001). All four cases of major complications occurred in the conventional group. Two cases with loosening and anterior angulation were treated with a change of prosthesis, and another with infection underwent amputation. The remaining case with loosening had conservative management. At the final follow-up, the average Musculosketal Tumor Society score of the allograft group (26.1) was better than that of the conventional group (20.9). Conclusion: Bone union in periprosthetic fractures of a tumor prosthesis can be achieved, but the minimization of complications is important. An onlay allograft facilitates firm fixation and increases the bone stock with a shortened time to union. This simple method can minimize the risk of loosening, joint contracture, and re-fracture.

Ecological Study on Poisonous Snake and Investigation of the Venom Characteristics, Snakebiting Frequenty in Korea (한국산 독사의 생태학적 특징 및 독성, 교상빈도에 관한 조사, 연구)

  • Shim, Jae-Han;Son, Young-Jong;Lee, Sang-Seob;Park, Kyung-Seok;Oh, Hee-Bok;Park, Young-Do
    • Korean Journal of Environment and Ecology
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    • v.12 no.1
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    • pp.58-77
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    • 1998
  • Four species(25%) of Viperidae(Agkistrodon brevicaudus, Agkistrodon ussuriensis, Agkistrodon saxatilis) and Cloubridae(Rhabdophis tigrenus tigrenus) were Korean poisonous snake. Copulation season of these species was from July to August. Reproduction mode of genus Agkistrodon species was ovoviviparous but Rhabdophis tigrinus tigrinus was the other pattern of oviparous. Optimal movement temperature range was from 20$\circ $C to 29$\circ $C(March~September). Wjen atmosphere temperature was below 10$\circ $C, at that time they hibernate at the ground, rock bottom, stone wall and embankment around the end of a field. The venom of these snakes consist mainly Hematoxin, Cytolysin, Neurotoxin and Cardiotoxin of poisonous liquids. These material injection to animal cause systemic syndrome such as Dizziness(25.7%), Vomitting(23.1%), Fever(22%), Visual trouble(18%), Headace(17.7%), Dyspnoea(17.6%) and bring about other local syndrome such as Discoloration(54.2%), Bleeding(20.2%), Bullae(10.7%) and Skin ulcer(!0.8%). The annual distribution was appeared to decrease 1972 after 1992 and average snakebiting patients was 25.6 per year, but practically total estimated snakebiting was 2,700 per year. The seasonal distribution was most frequent in August(25%), and mortality was 1.8%(26 per 1,430). The sex ratio was 2:1 and according to age distribution, it was most prevalent at one's fifties(19%). The most frequent place where the accident happened was the field(48.2%) and most predilection site of the body for victim were hand(47.8%) and foot(39.5%), Commonly bite snake were Agkistrodon ussuriensis(27.1%), Agkistrodon brevicaudus(22.6%) and Agkistrodon saxatilis(9.6%) but 40.7% of species could not be identified. Treatment of antivenin patient was 75.9% (1,068/1,407).

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Selection and Validation of an Analytical Method for Trifludimoxazin in Agricultural Products with LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Trifludimoxazin의 시험법 선정 및 검증)

  • Sun Young Gu;Su Jung Lee;So eun Lee;Chae Young Park;Jung Mi Lee;Inju Park;Yun Mi Chung;Gui Hyun Jang;Guiim Moon
    • Journal of Food Hygiene and Safety
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    • v.38 no.3
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    • pp.79-88
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    • 2023
  • Trifludimoxazin is a triazinone herbicide that inhibits the synthesis of protoporphyrinogen oxidase (PPO). The lack of PPO damages the cell membranes, leading to plant cell death. An official analytical method for the safety management of trifludimoxazin is necessary because it is a newly registered herbicide in Korea. Therefore, this study aimed to develop a residual analysis method to detect trifludimoxazin in five representative agricultural products. The EN method was established as the final extraction method by comparing the recovery test and matrix effect with those of the QuEChERS method. Various sorbent agents were used to establish the clean-up method, and no differences were observed among them. MgSO4 and PSA were selected as the final clean-up conditions. We used LC-MS/MS considering the selectivity and sensitivity of the target pesticide and analyzed the samples in the MRM mode. The recovery test results using the established analysis method and inter-laboratory validation showed a valid range of 73.5-100.7%, with a relative standard deviation and coefficient of variation less than 12.6% and 14.5%, respectively. Therefore, the presence of trifludimoxazin can be analyzed using a modified QuEChERS method, which is widely available in Korea to ensure the safety of residual insecticides.

Development of Analytical Method for Detection of Fungicide Validamycin A Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Validamycin A의 시험법 개발)

  • Park, Ji-Su;Do, Jung-Ah;Lee, Han Sol;Park, Shin-min;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.1
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    • pp.22-29
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    • 2019
  • Validamycin A is an aminoglycoside fungicide produced by Streptomyces hygroscopicus that inhibits trehalase. The purpose of this study was to develop a method for detecting validamycin A in agricultural samples to establish MRL values for use in Korea. The validamycin A residues in samples were extracted using methanol/water (50/50, v/v) and purified with a hydrophilic-lipophilic balance (HLB) cartridges. The analyte was quantified and confirmed by 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 (0.005~0.5 ng) into a blank extract with $R^2$ > 0.99. The limits of detection and quantification were 0.005 and 0.01 mg/kg, respectively. For validation validamycin A, recovery studies were carried out three different concentration levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) with five replicates at each level. The average recovery range was from 72.5~118.3%, with relative standard deviation (RSD) less than 10.3%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the NIFDS (National Institute of Food and Drug Safety) guideline (2016). Therefore, the proposed analytical method is accurate, effective and sensitive for validamycin A determination in agricultural commodities.

Development and Validation of the Analytical Method for Oxytetracycline in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 Oxytetracycline의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, ong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.227-234
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    • 2019
  • An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.

Studies on Inheritance and Ecological Variation of the Culm Length and Its Related Characters in Short-Statured Rice Varieties (수도단간품종의 간장 및 관련형질의 유전과 생태적 변이에 관한 연구)

  • Sung-Ho Bea
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.13
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    • pp.1-40
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    • 1973
  • These studies were aimed at clarification of genetic and ecological variation in culm length, panicle length and plant height of the $\textrm{F}_2$ plants in some selected crosses made between semi-dwarf rice varieties and tall Japonica ones. One Indica semi-dwarf, Taichung Native 1, one Indica $\times$ Japonica hybrid, IE51 and one Japonica semi-dwarf, Tankanbaekmang were used as short-gene donors while two of medium maturity varieties, Jinheung and Kwanok and one late veriety, Palkweng were used as the corresponding counterpart of respective dwarf varieties in a series of crosses. Five different crosses, Kwanok $\times$ Tankanbaekmang, Palkweng $\times$ Tankanbaekmang, Jinheung $\times$ T(N)1, Kwanok $\times$ T(N)1 and Kwanok $\times$ IE51, were made among the above six varieties. The $\textrm{F}_2$ plants of these crosses together with the concerned parental varieties were grown under several different conditions including three levels of each nitrogen and planting space, three planting seasons and three locations in 1968, to investigate variation in length of culm and panicle, and plant height. On the other hand, the F$_3$ progenies which were derived from the shortest 10 percent of the plants of three $\textrm{F}_2$ populations, Kwanok $\times$ T(N)1, Jinheung $\times$ T(N) 1 and Kwanok $\times$ IE51 grown in the previous year, were compared each other on the basis of selection efficiency in culm length. The experimental results could be summarized as follows; 1. Genetic behavior A. It was revealed that Tankanbaekmang, one of Japonica dwarf has a simple recessive gene responsible for short culm expression, showing a typical segregation ratio of three tall to one short culm plants in $\textrm{F}_2$ generation of the crosses either with Kwanok or Palkweng. B. In the both combinations, segregation pattern of the panicle length was exactly same as that of culm length. It seems that the same gene controls both culm length and panicle length. C. No difference between segregation of culm length and plant height in the above crosses was observed. D. T(N)1, one of Indica semi-dwarf did not show such a simple genetic behavior as detected from the crosses with Tankanbaekmang in segregation of culm length but formed a continuous and normal distribution curve. Therefore, some nonallelic genic actions might be involved in expression of culm length of the counterpart varieties of T(N)1. In particular, a transgressive segregation appeared toward the direction of longer culm length in case of Jinheung $\times$ T(N)1. The genetic behavior of panicle length and plant height generally coincided with that of culm length in all the cases. E. IE51 demonstrated exactly the same genetic behavior as that of T(N)1 when this variety was crossed with Kwanok. It was clearly clarified that the simple recessive gene controlling dwarfism from T(N)1 was well incorporated into this variety. 2. Ecological variation A. In general, there was a decreasing tendency in culm length and plant height of rice plant as seeding delayed while it was not so noticeable in panicle length. The decreasing magnitude varied from variety to variety and from cross to cross. Genetic behavior of the culm length and related characters of these materials was not disturbed by the variation of seeding season, nitrogen level, planting space and experimental location. E. The elongation mode of the upper three internodes was very similar to the segregation mode of culm length, panicle length and plant height in $\textrm{F}_2$ populations of . all the crosses investigated in this study. Accordingly, this result confirmed that the roles of the upper three internodes are very important in manifesting plant stature in rice. C. The effect of nitrogen on culm length and the related other two characters seemed to be meager. However, it was true to show an increasing tendency of those characters as nitrogen level got increased from 4 kg to 12kg per l0a, with different magnitude depending upon variety or cross. D. Also, the effect of planting space on culm length, panicle length and plant height was relatively small in all the cases. Those characters varied again depending upon variety or cross. However, a general increasing tendency was detected in manifestation of those traits under denser planting space condition. E. All the parental varieties produced shorter culm, panicle and plant height when they were grown at the lower latitude locations. It might be attributed to the fact that their reproductive growth accelerated with increased temperature prevailing at the lower latitude locations such as Iri and Mi1yang. On the countrary, $\textrm{F}_2$ population reacted differently to the different locations from the parental varieties. All the $\textrm{F}_2$ plants produced the longest culm, panicle and plant at Milyang. 3. Selection efficiency A. The heritability of culm length in Kwanok $\times$ T(N)1, Kwanok $\times$ IE51 and Jinheung$\times$T(N)1 was 92 percent, 74 percent and 55 percent, respectively. B. The actual genetic advance for culm length obtained from the progeny lines of the selected plants(10 precent) from the $\textrm{F}_2$ generation, was comparable to the expected advance calculated from the original $\textrm{F}_2$ populations. As compared with the $\textrm{F}_2$ population, the $\textrm{F}_3$ plants of Kwanok $\times$ T(N)l shortened on the average by 20.8cm, those of Kwanok $\times$ IE51 did 8.7cm and those of Jinheung$\times$T(N)1 20.0cm, respectively. C. Panicle length of the populations was differently affected from one cross to another by the selection based upon culm length in $\textrm{F}_2$ Kwanok $\times$ T(N)1 did not show any noticeable shortening of its culm length due to the selection pressure. On the other hand, both Kwanok $\times$ IE51 and Jinheung $\times$ T(N)1 showed a considerable shortening of their panicles in case of selection for culm length. Based upon the above results, it could be concluded that the ecological variation in culm length, panicle length and plant height was relatively small and fallen within the range of genetic variation. Considering from the fact that the simple recessive gene governing short height of Tankanbaekmang always accompanied with some undesirable characters such as short panicle and extremely small grain, the short gene of T(N)1 seemed to be more useful as dwarf gene source since it did not carry short gene together with such undesirable traits.

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Assessment of Bone Metastasis using Nuclear Medicine Imaging in Breast Cancer : Comparison between PET/CT and Bone Scan (유방암 환자에서 골전이에 대한 핵의학적 평가)

  • Cho, Dae-Hyoun;Ahn, Byeong-Cheol;Kang, Sung-Min;Seo, Ji-Hyoung;Bae, Jin-Ho;Lee, Sang-Woo;Jeong, Jin-Hyang;Yoo, Jeong-Soo;Park, Ho-Young;Lee, Jae-Tae
    • Nuclear Medicine and Molecular Imaging
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    • v.41 no.1
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    • pp.30-41
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    • 2007
  • Purpose: Bone metastasis in breast cancer patients are usually assessed by conventional Tc-99m methylene diphosphonate whole-body bone scan, which has a high sensitivity but a poor specificity. However, positron emission tomography with $^{18}F-2-deoxyglucose$ (FDG-PET) can offer superior spatial resolution and improved specificity. FDG-PET/CT can offer more information to assess bone metastasis than PET alone, by giving a anatomical information of non-enhanced CT image. We attempted to evaluate the usefulness of FDG-PET/CT for detecting bone metastasis in breast cancer and to compare FDG-PET/CT results with bone scan findings. Materials and Methods: The study group comprised 157 women patients (range: $28{\sim}78$ years old, $mean{\pm}SD=49.5{\pm}8.5$) with biopsy-proven breast cancer who underwent bone scan and FDG-PET/CT within 1 week interval. The final diagnosis of bone metastasis was established by histopathological findings, radiological correlation, or clinical follow-up. Bone scan was acquired over 4 hours after administration of 740 MBq Tc-99m MDP. Bone scan image was interpreted as normal, low, intermediate or high probability for osseous metastasis. FDG PET/CT was performed after 6 hours fasting. 370 MBq F-18 FDG was administered intravenously 1 hour before imaging. PET data was obtained by 3D mode and CT data, used as transmission correction database, was acquired during shallow respiration. PET images were evaluated by visual interpretation, and quantification of FDG accumulation in bone lesion was performed by maximal SUV(SUVmax) and relative SUV(SUVrel). Results: Six patients(4.4%) showed metastatic bone lesions. Four(66.6%) of 6 patients with osseous metastasis was detected by bone scan and all 6 patients(100%) were detected by PET/CT. A total of 135 bone lesions found on either FDG-PET or bone scan were consist of 108 osseous metastatic lesion and 27 benign bone lesions. Osseous metastatic lesion had higher SUVmax and SUVrel compared to benign bone lesion($4.79{\pm}3.32$ vs $1.45{\pm}0.44$, p=0.000, $3.08{\pm}2.85$ vs $0.30{\pm}0.43$, p=0.000). Among 108 osseous metastatic lesions, 76 lesions showed as abnormal uptake on bone scan, and 76 lesions also showed as increased FDG uptake on PET/CT scan. There was good agreement between FDG uptake and abnormal bone scan finding (Kendall tau-b : 0.689, p=0.000). Lesion showed increased bone tracer uptake had higher SUVmax and SUVrel compared to lesion showed no abnormal bone scan finding ($6.03{\pm}3.12$ vs $1.09{\pm}1.49$, p=0.000, $4.76{\pm}3.31$ vs $1.29{\pm}0.92$, p=0.000). The order of frequency of osseous metastatic site was vertebra, pelvis, rib, skull, sternum, scapula, femur, clavicle, and humerus. Metastatic lesion on skull had highest SUVmax and metastatic lesion on rib had highest SUVrel. Osteosclerotic metastatic lesion had lowest SUVmax and SUVrel. Conclusion: These results suggest that FDG-PET/CT is more sensitive to detect breast cancer patients with osseous metastasis. CT scan must be reviewed cautiously skeleton with bone window, because osteosclerotic metastatic lesion did not showed abnormal FDG accumulation frequently.