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Analysis of Zearalenone Contamination in Cereal-Based Products Using High Performance Liquid Chromatography-Fluorescence Detector and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry (곡류가공품 중 제랄레논 오염도 조사)

  • Jang, Mi-Ran;Lee, Chang-Hee;Choi, In-Sun;Shin, Choon-Shik;Kim, Jin-Hee;Jang, Young-Mi;Kim, Dong-Sul;Ahn, Dong-Hyun
    • Korean Journal of Food Science and Technology
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    • v.43 no.2
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    • pp.224-229
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    • 2011
  • Zearalenone (ZEA) is an estrogenic mycotoxin mainly produced by Fusarium graminerum, a species which colonizes a wide variety of cereals, including wheat, barley and processed products. A survey of ZEA contamination was conducted on 141 dried confectioneries, 59 breads and rice cakes, 135 noodles and 101 other products, for a total of 432 commercial samples. Samples were analyzed by high performance liquid chromatography with fluorescence detection (HPLC-FLD) after immunoaffinity clean-up and was confirmed by liquid chromatography tandem mass spectrometry (LCMS/MS). The limits of detection and quantification were 2.0 and $6.0{\mu}g/kg$, respectively. The recovery ranged from 80.2% to 98.4% in the cereal based product. ZEA was detected in 38 samples (8.8% incidence), including 3 snack, 2 biscuit and 33 other cereal products. The ZEA contamination levels were in the range of $5.38-53.76{\mu}g/kg$. Finally, LC-MS/MS analysis of the contaminated samples was conducted to confirm the detected ZEA, and all 38 samples showing ZEA by HPLC-FLD were confirmed by LC-MS/MS.

Optimization of Extraction Method for the Quantitative Analysis of Gallic Acid from Cornus officinallis (산수유로부터 gallic acid 추출 및 HPLC에 의한 정량분석)

  • Jang, Mi;Kim, Yeon-Ju;Min, Jin-Woo;Yang, Deok-Chun
    • Korean Journal of Food Science and Technology
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    • v.41 no.5
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    • pp.498-502
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    • 2009
  • Cornus fructus has been used as a tonic, astringent, and haemostatic agent in Korea, China, and Japan. In this study, the fruit of Cornus officinalis was treated with different osmotic pressures, pH values, heat, and ethanol percentages in order to establish optimum extraction conditions for gallic acid, an example of a hydrolyzable tannin. The extract was analyzed by HPLC and LC-MS/MS to identify the gallic acid. As a result, the highest extraction rate of gallic acid (1.57 mg/g) occurred when the Cornus fructus was extracted with 100% ethanol for 1 hr at $80^{\circ}C$. Also, when it was treated with 70% ethanol for 24 and 48 hr, contents of gallic acid were 1.35 and 1.50 mg/g, respectively.

Long-Term Treatment Results in Soft Tissue Sarcomas of the Thoracic Wall Treated with Pre-or-Postoperative Radiotherapy - a Single Institution Experience

  • Oksuz, Didem Colpan;Ozdemir, Sevim;Kaydihan, Nuri;Dervisoglu, Sergulen;Hiz, Murat;Tuzun, Hasan;Mandel, Nil Molinas;Koca, Sedat;Dincbas, Fazilet Oner
    • Asian Pacific Journal of Cancer Prevention
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    • v.15 no.22
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    • pp.9949-9953
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    • 2014
  • Objective: To evaluate the long term results among patients with soft tissue sarcoma of the thoracic wall. Materials and Methods: Twenty-six patients who were treated with pre-or postoperative radiotherapy between December 1980-December 2007, with a diagnosis of soft tissue sarcoma of the thoracic wall were retrospectively evaluated. Results: The median age was 44 years (14-85 years) and 15 of them were male. A total of 50% of patients were grade 3. The most common histologic type of tumor was undifferentiated pleomorphic sarcoma (26.9%). Tumor size varied between 2-25 cm (median 6.5 cm). Seventeen of the cases had marginal and 9 had wide local resection. Four cases received preoperative radiotherapy and 22 postoperative radiotherapy. Six of the patients with large and high grade tumors received chemotherapy. Median follow-up time was 82 months (9-309 months). Local recurrence and metastasis was detected in 34.6% and 42.3% of patients, respectively. Five-year local control (LC), disease-free survival (DFS), overall survival (OS), and disease-specific survival (DSS) were 62%, 38%, 69%, and 76% respectively. On univariate analysis, the patients with positive surgical margins had a markedly lower 5-year LC rate than patients with negative surgical margin, but the difference was not significant (43% vs 78%, p=0.1). Five-year DFS (66% vs 17%) and DSS (92% vs 60%) rates were significantly worse for the patients who had high grade tumors (p=0.01, p=0.008 respectively). Conclusions: Tumor grade and surgical margin are essential parameters for determining the prognosis of thoracic wall soft tissue sarcoma both in our series and the literature.

Method Development and Validation for Analysis of Isopyrazam Residues in Agricultural Products (농산물 중 살균제 Isopyrazam의 개별 잔류분석법 확립)

  • Kim, Ji-Yoon;Kim, Ja-Young;Ham, Hun-Ju;Do, Jung-Ah;Oh, Jae-Ho;Lee, Young-Deuk;Hur, Jang-Hyun
    • The Korean Journal of Pesticide Science
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    • v.17 no.2
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    • pp.84-93
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    • 2013
  • Validated analytical methods for isopyrazam are meager or lacking. In the present study, a single residual analytical method was developed for isopyrazam in selected commodities. Isopyrazam was analyzed in brown rice, soybean, green pepper, mandarin, cucumber, and Korean melon. We tried different solvents and methods through extraction, partition and purification steps to obtain best analytical results. For isopyrazam samples were extracted with acetonitrile, concentrated and partitioned with n-hexane, clean-up using florisil with n-hexane/ethylacetate (70/30) and analyzed with HPLC/UVD. The limit of quantitation (LOQ) for isopyrazam was 1.0 ng (S/N > 10) and method LOQ (MLOQ) was 0.04 mg $kg^{-1}$. Recovery ranged through 81.0~105.3% (syn-isomer) and 80.8~105.6% (anti-isomer) at fortification level of 0.04 (MLOQ), 0.4 (10 ${\times}$ MLOQ), and 2.0 (50 ${\times}$ MLOQ). The coefficient of variation (CV) for isopyrazam was less than 10% regardless of sample types. These results were further confirmed with LC/MS, respectively. The proposed method is highly reproducible and sensitive and is suitable for routine analysis.

Establishment of Pre-Harvest Residue Limit (PHRL) of Emamectin benzoate during Cultivation of Amaranth (생산단계 비름 중 Emamectin benzoate의 잔류허용기준 설정)

  • Kim, Kyung Jin;Kim, Da Som;Heo, Seong Jin;Ham, Hun Ju;Hur, Jang Hyun
    • The Korean Journal of Pesticide Science
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    • v.17 no.2
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    • pp.77-83
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    • 2013
  • This study was performed to investigate pre-harvest residue limit (PHRL) in amaranth, to estimate biological half-life of emamectin benzoate and identify the characteristics of the residue. Pesticides of standard and double appplication rate, were sprayed once on amaranth at 0, 1, 2, 3, 5, 7, 10, 14 days before harvest. Amaranth sample was extracted with acetonitrile and partitioned with dichloromethane, and pesticide residues were determined with LC/MS/MS. The limit of detection of emamectin benzoate was 0.01 mg/kg. Recoveries of emamectin benzoate ($B_{1a}$, $B_{1b}$) at two fortification levels of 0.1 and 0.5 mg/kg, $B_{1a}$ were $93.3{\pm}0.7%$ and $93.2{\pm}7.7%$, $B_{1b}$ were $106.6{\pm}1.9%$ and $80.5{\pm}6.6%$, respectively. The biological half-lives of emamectin benzoate were about 2.0 days at standard application rate and 1.7 days at double application rate, respectively. The PHRL of emamectin benzoate were recommended as 0.84 mg/kg for 10 days before harvest.

Analytical Method of Bentazone Residue in Agricultural Commodities Using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 농산물 중 bentazone의 분석법 확립)

  • Kim, Young-Hak;Lee, Su-Jin;Song, Lee-Seul;Hwang, Young-Sun;Lee, Young-Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.15 no.2
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    • pp.149-159
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    • 2011
  • Bentazone is benzothiadiazole group herbicide, and used to foliage treatment. This herbicide have already been widely used for cereals and vegetables planting in worldwide. This experiment was conducted to establish a determination method for bentazone residue in crops using HPLC-UVD/MS. Bentazone residue was extracted with acetone (adjusted pH 1 with phosphoric acid) from representative samples of five raw products which comprised hulled rice, soybean, apple, green pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover bentazone from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The bentazone was quantitated by HPLC with UVD, using a YMC ODS AM 303 ($4.6{\times}250$ mm) column. The crops were fortified with bentazone at 3 levels per crop. Mean recovery ratio were ranged from 82.0% for a 0.2 mg/kg in apple to 97.9% for a 0.02 mg/kg in Chinese cabbage. The coefficients of variation were ranged from 0.5% for a 0.02 mg/kg in soybean to 9.7% for a 0.02 mg/kg in Chinese cabbage. Quantitative limit of bentazone was 0.02 mg/kg in representative five crop samples. A LC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of bentazone in agricultural commodities.

New Liquid Crystal-Embedded PVdF-co-HFP-Based Polymer Electrolytes for Dye-Sensitized Solar Cell Applications

  • Vijayakumar, G.;Lee, Meyoung-Jin;Song, Myung-Kwan;Jin, Sung-Ho;Lee, Jae-Wook;Lee, Chan-Woo;Gal, Yeong-Soon;Shim, Hyo-Jin;Kang, Yong-Ku;Lee, Gi-Won;Kim, Kyung-Kon;Park, Nam-Gyu;Kim, Suhk-Mann
    • Macromolecular Research
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    • v.17 no.12
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    • pp.963-968
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    • 2009
  • Liquid crystal (LC; E7 and/or ML-0249)-embedded, poly(vinylidenefluoride-co-hexafluoropropylene) (PVdF-co-HFP)-based, polymer electrolytes were prepared for use in dye-sensitized solar cells (DSSCs). The electrolytes contained 1-methyl-3-propylimidazolium iodide (PMII), tetrabutylammonium iodide (TBAI), and iodine ($I_2$), which participate in the $I_3^-/I^-$ redox couple. The incorporation of photochemically stable PVdF-co-HFP in the DSSCs created a stable polymer electrolyte that resisted leakage and volatilization. DSSCs, with liquid crystal(LC)-embedded PVdF-co-HFP-based polymer electrolytes between the amphiphilic ruthenium dye N719 absorbed to the nanocrystalline $TiO_2$ photoanode and the Pt counter electrode, were fabricated. These DSSCs displayed enhanced redox couple reduction and reduced charge recombination in comparison to that fabricated from the conventional PVdF-co-HFP-based polymer electrolyte. The behavior of the polymer electrolyte was improved by the addition of optimized amounts of plasticizers, such as ethylene carbonate (EC) and propylene carbonate (PC). The significantly increased short-circuit current density ($J_{sc}$, $14.60\;mA/cm^2$) and open-circuit voltage ($V_{oc}$, 0.68 V) of these DSSCs led to a high power conversion efficiency (PCE) of 6.42% and a fill factor of 0.65 under a standard light intensity of $100\;mW/cm^2$ irradiation of AM 1.5 sunlight. A DSSC fabricated by using E7-embedded PVdF-co-HFP-based polymer electrolyte exhibited a maximum incident photon-to-current conversion efficiency (IPCE) of 50%.

Analytical Method for Flusulfamide as Benzenesulfonamide Fungicide, Residues in Major Agricultural Commodities (주요 농산물 중 Bezenesulfonamide계 살균제 Flusulfamide의 잔류 분석법)

  • Ahn, Kyung-Geun;Kim, Gi-Ppeum;Hwang, Young-Sun;Kang, In-Kyu;Lee, Young Deuk;Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
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    • v.37 no.1
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    • pp.57-65
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    • 2018
  • BACKGROUND: An analytical method was developed using HPLC-UVD/MS to precisely determine the residue of flusulfamide, a benzenesulfonamide fungicide used to inhibit spore germination. METHODS AND RESULTS: Flusulfamide residue 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 large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives 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 an octadecylsilyl column in HPLC, flusulfamide was successfully separated from co-extractives of sample, and sensitively quantitated by ultraviolet absorption at 280 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop sample fortified with flusulfamide at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries ranged from 82.3 to 98.2% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of flusulfamide was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue.

A STUDY ON THE EFFECT OF BASE MATERIALS TO PROTECT THE CERVICAL LEAKAGE OF BLEACHING AGENTS (표백제의 치경부 누출을 방지하기 위한 각종 이장재의 효과에 관한 연구)

  • Song, Byeong-Choon;Cho, Young-Gon
    • Restorative Dentistry and Endodontics
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    • v.19 no.2
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    • pp.585-601
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    • 1994
  • The purpose of this study was to evaluate the ability of several intracoronal base materials to prevent cervical leakage of a bleaching agent into the dentinal tubules and along the root canal. In this study, thirty-two anterior teeth were used. After lingual access was prepared in each tooth, tooth was instrumented with a step-back technique to a Nos. 40-50 using K-type files. All teeth were obturated with a lateral condensation technique. Excess gutta percha was removed with a warm instrument to the facial level of the CEJ. Teeth were divided into four groups : Teeth in control group were not filled with base material. Teeth in groups 1, 2, and 3 had 2mm of gutta percha removed with a warm instrument, then Dycal, Fuki II LC and Z-100 were filled with palstic instruments on the top of the gutta percha respectively. All teeth were bleached for 7 days, fresh bleach was added for another 7 days, then a 10 % methylene blue dye was placed inside the access preparation. They were stored at $37^{\circ}C$ and $100^{\circ}C$ humidity for 5 days. Each tooth was sectioned perpendicular to the long axis using a diamond disk. Initial cuts were made at the most coronal level of facial and lingual CEJ's, then another cuts continued appically in the levels of 0.5mm, 1.5mm, and 2.0mm respectively. The amount of dye leakage through the dentinal tubules was determined at each cut section. In addition, when the cut specimen was determined to be last penetration of any dye, this level was recorded as depth of apical leakage from the coronal terminus of the gutta percha, Dycal, Fuji II LC and Z-100. The acquired data were analyzed by Tukey's Multiple Range Test adn Cochran-Mantel-Haenszel Test to see if there was any statistically significant difference in dye penetration and linear apical leakage among the groups. The results were as follows : 1. Control group at levels of CEJ and 0.5mm, group 3 at level of 1.5mm, and group 2 AND 3 at level of 2.0mm showed the least dye penetration through the facial or lingual dentinal tubules, but there were no significant difference among three groups. 2. Group 2 at levels of CEJ and 0.5mm, group 3 at level of 1.5mm, and group 2 and 3 at level of 2.0mm showed the least dye penetration through the proximal dentinal tubules, but there were no significant difference among control group, group 2, and group 3. 3. Group 1 showed the greatest dye penetration through the facial or lingual and proximal dentinal tubules at all levels, and there were significant difference with other three groups. 4. Control group and group 1 showed 2mm apical dye leakage at facial or lingual and proximal aspects, group 2 showed 1.5mm, and group 3 showed 0.5mm.

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Control effects of 20 chemical insecticides and new strains of Bacillus thuringiensis against the fungus gnat (Bradysia difformis, Sciaridae, Diptera)

  • Jang, Hyun-Ju;Kim, Hee-Ji;Kwon, Hye-Ri;Yu, Yong-Man;Youn, Young-Nam
    • Korean Journal of Agricultural Science
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    • v.45 no.2
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    • pp.185-196
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    • 2018
  • The fungus gnat, Bradysia difformis, damages various crops in greenhouses and is recognized as an important pest around the world. Additionally, in the future, many other greenhouse crops will be added to the list of crops damaged by the fungus gnat. In this study, to find effective control methods for the fungus gnat, the insecticidal effect of 20 chemical synthetic insecticides was tested with the potato disc and pot treatment methods; additionally, the control effect of 16 strains of B. thuringiensis was examined with the potato disk method. The fungus gnat larvae were treated for 2 days with each of the synthetic insecticides to determine insecticidal effect using the potato disc method. The results were as follows. Among the highly insecticidal active pesticides, chlorfenapyr exhibited a 100% insecticidal activity, and fenazaquin, acetamiprid, dinotefuran, fenthion and thiamethoxam exhibited more than a 90% insecticidal activity. For the pot treatment method, chlorfenapyr exhibited a 3.3% insecticidal effect, and thiamethoxam, acetamiprid, dinotefuran, fenthion, etc. exhibited an insecticidal effect of less than 10% of the emergence rate to adult fungus gnat after 14 days of treatment. To select the B. thuringiensis strains that have an insecticidal effect on the fungus gnat, 16 strains were biologically assayed using the potato disc method. Among the 16 strains, Bt-3, Bt-8 and Bt-13 had more than a 70% insecticidal effect. The $LC_{50}$ and $LC_{95}$ values of Bt-3, Bt-8 and Bt-13 were $3.7{\times}10^5$ and $4.7{\times}10^8cfu/ml$, $1.4{\times}10^5$ and $1.1{\times}10^7cfu/ml$, and $1.4{\times}10^5$ and $1.3{\times}10^7cfu/ml$, respectively.