• Title/Summary/Keyword: LC20

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Simultaneous Analytical Method for the Neomycin, Gentamicin Residues in Seafood (수산물 중 네오마이신, 겐타마이신 동시분석법 개발)

  • Hong, Young-Min;Lee, Seok-Ki;Kim, Hyoung-Ah;Hwang, Yu-Kyung
    • Journal of Applied Biological Chemistry
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    • v.53 no.1
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    • pp.25-30
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    • 2010
  • This paper describes a simultaneous method for the determination of two aminoglycosides (neomycin and gentamicin) using solid phase extraction followed by liquid chromatograph-mass spectrometry. The extract was applied to an WCX and HLB solid phase extraction cartridge. The cartridges were washed with water and methanol, and analytes were eluted with TCA buffer-acetonitrile mixture. The aminoglycosides were separated by ion-pairing reversed phase mode prior to ESI-LC/MS. Under the conditions applied neomycin was almost separated from all the gentamicin compounds. No interfering peaks from endogenous compounds of matrix were noted at the elution position of the analytes. Recoveries of neomycin fortified at levels of 0.25, 0.5, 1.0 and 2.0 mg/kg seafood samples ranged from 92 to 115%. Recoveries of gentamycin fortified at levels of 0.05, 0.1, 0.2, 0.4 mg/kg seafood samples ranged from 99 to 116%. Method detection limits in four seafood sample matrices were between 0.002 and 0.033 mg/kg.

A Study on the Evaluation of Teratogenecity of Chemical by Korean Brown Frog Embryo, Rana dybowskii (산개구리 배아를 활용한 화학물질의 기형성 평가에 관한 연구)

  • Ko Sun-Kun
    • Korean Journal of Environment and Ecology
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    • v.18 no.3
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    • pp.333-339
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    • 2004
  • The Frog Embryo Teratogenesis Assay-Xenopus(FETAX) protocol was recently adopted as a valuable tool fur evaluating chemical toxicity and the effect of environmental contaminants in frogs. In this study, the teratogenecity of NiCl$_2$, Carbofuran, Diazinon were determined in the Korean frog, Rana dybowskii using the FETAX protocol. The mortality rate and the percentage of malformed larvae were investigated by probit analysis, The teratogenic concentrations(EC$_{50}$) of NiCl$_2$, Carbofuran and Diazinon were 0.4 and 1.6 and 1.9 mg/1. The embryolethal concentrations(LC$_{50}$) of NiCl$_2$, Carbofuran and Diazinon were 17.6 and 41.5 and 20.2mg/1. The teratogenic indices (TI=LC$_{50}$/EC$_{50}$) were 43.8 for NiCl$_2$, 26.0 for Carbofuran and 10.6 for Diazinon. NiCl$_2$, Carbofuran and Diazinon were shown to be potent teratogens for Rana dybowskii embryo, causing concentration related increase of edema, tail and abdomen. The study results reveal that NiCl$_2$, Carbofuran and Diazinon suppress the development of embryos at relatively low concentrations. Therefore, the Rana dybowskii embryo teratogenesis assay system was proven to be a useful tool to evaluate the toxicity of environmental pollutants.lutants.

Simultaneous Determination of Aflatoxins and Ochratoxin A in Pork by LC-MS/MS (LC-MS/MS를 이용한 돼지고기 중 총아플라톡신 및 오크라톡신 A 동시분석법 확립)

  • Paek, Ockjin;Park, Songyi;Park, Ki Hun;Kim, Sheen-Hee;Suh, Saejung;Yoon, Hae Jung
    • Journal of Food Hygiene and Safety
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    • v.31 no.3
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    • pp.194-200
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    • 2016
  • Aflatoxins and ochratoxin A (AFTs and OTA) are secondary fungal metabolites produced by several moulds, mainly by Aspergillus flavus by Aspergillus ochraceus and Penicillium verrucosum, and these toxins can be transferred to animals and humans through the ingestion of contaminated feed and food. This study was to develop the analytical method for determination the levels of AFTs ($B_1$, $B_2$, $G_1$ and $G_2$) and OTA in pork. The AFTs and OTA were analyzed simultaneously by electrospray ionization in positive ion mode and mass reaction monitoring (MRM) after solid phase extract (SPE) columns clean-up. Performance characteristics, such as accuracy, precision, linear range, limit of detection (LOD) and quantification (LOQ), were also determined. Matrix-matched standard calibration was used for quantification, obtaining the recoveries in the range of 67.3~108.2% with the relative standard deviations of < 20%. Limits of detection and quantification were also estimated, obtaining the limits of quantification ranged in $0.7{\sim}1.3{\mu}g/kg$. The results of the inter-day study, which was performed with pork samples for 3 days, showed an accuracy of 92.0~109.9%. The precisions (expressed as relative standard deviation values) for the inter day variation were 2.6~17.8%. The method developed in this study was able to carry out the analysis with the satisfactory intensity and accuracy.

The Optimum Addition Ratio of Nano Hydroxyapatite to Glass Ionomer Dental Cement (Changes in Demineralization Resistance and Bonding Strength of Light Cured Glass Ionomer after the Addition of Nano Hydroxyapatite in Various Ratio) (글래스아이오노머에 대한 나노 하이드록시아파타이트의 최적 첨가 비율(나노 하이드록시아파타이트의 첨가 비율에 따른광중합형 글래스아이오노머의 결합강도와 탈회저항성의 변화 비교))

  • Kim, Nam Hyuk;Kim, Seong Oh;Song, Je Seon;Lee, Jae Ho;Son, Heung Kyu;Choi, Byung Jai;Choi, Hyung Jun
    • Journal of the korean academy of Pediatric Dentistry
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    • v.40 no.3
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    • pp.159-167
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    • 2013
  • The aim of this study was to evaluate changes in demineralization resistance and bonding strength of light cured glass ionomer after the addition of nano hydroxyapatite in various ratios. Fuji II LC GIC (GC Co., Japan) was used as the control group and also as a base material for experimental group. HA was mixed into the RMGIC at various ratio to create a HA-LC GIC mixture, preparing six experimental groups, i.e. 5%, 10%, 15%, 20%, 25%, 30% HA-LC GIC. According to the results, the bonding strength increased due to the addition of HA, showing the maximum value at the 15% nano HA group (p < 0.05). Under CLSM observation after 4 days of demineralization, the HA groups were more resistant to demineralization compared to the control group. No significant difference was observed between HA groups. In analysis through SEM, the HA groups showed attachment of granular materials and decreased demineralized tooth surfaces under influence of HA particles.

Comparison of Physicochemical Properties between Extracts and Soaked Liquor of Lespedeza cuneata G.Don (비수리(Lespedeza cuneata G.Don) 추출물과 담금주의 이화학적 특성비교)

  • Jeong, Kap-Seop
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.18 no.12
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    • pp.705-711
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    • 2017
  • Lespedeza cuneata (LC) is a herbaceous plant that grows throughout Korea. To investigate the physicochemical properties and the antioxidant activities of LC extracts and LC-soaked liquor (s. liquor), extraction with distilled water (DW) and ethanol was conducted and the extracts were compared with s. liquor. A total of 22 free amino acids from LC extract were detected, with the main ones being phosphoethanolamine 20.36>L-proline 18.02>ammonia 14.48>L-aspartic acid 12.96>${\gamma}$-amino-n-butyric acid 10.67%. The total flavonoid contents (TFC) and total phenolics contents (TPC) were in the order of s. liquor>DW>ethanol extract. The electron donating ability based on DPPH radical scavenging ability was highest for s.liquor, which equivalents 81.4% ascorbic acid in the order of s. liquor>ethanol>DW extract. The orders of ferric reducing antioxidant power and ABTS radical scavenging ability were proportional to the TFC and TPC of extracts, and in the order of s. liquor>ethanol>DW extract. The nitrite scavenging ability of s. liquor was highest among the three extracts (96.6% at pH 1.2), which was 2.6 times greater than that of DW extract.

Study on predicting the commercial parts discontinuance using unstructured data and artificial neural network (상용 부품 비정형 데이터와 인공 신경망을 이용한 부품 단종 예측 방안 연구)

  • Park, Yun-kyung;Lee, Ik-Do;Lee, Kang-Taek;Kim, Du-Jeoung
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.10
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    • pp.277-283
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    • 2019
  • Advances in technology have allowed the development and commercialization of various parts; however this has shortened the discontinuation cycle of the components. This means that repair and logistic support of weapon system which is applied to thousands of part components and operated over the long-term is difficult, which is the one of main causes of the decrease in the availability of weapon system. To improve this problem, the United States has created a special organization for this problem, whereas in Korea, commercial tools are used to predict and manage DMSMS. However, there is rarely a method to predict life cycle of parts that are not presented DMSMS information at the commercial tools. In this study, the structured and unstructured data of parts of a commercial tool were gathered, preprocessed, and embedded using neural network algorithm. Then, a method is suggested to predict the life cycle risk (LC Risk) and year to end of life (YTEOL). In addition, to validate the prediction performance of LC Risk and YTEOL, the prediction value is compared with descriptive statistics.

Analysis of Systemic Pesticide Imidacloprid and Its Metabolites in Pepper using QuEChERS and LC-MS/MS (QuEChERS 전처리와 LC-MS/MS를 이용한 고추 중 침투성농약 Imidacloprid 및 대사물질 동시분석법)

  • Seo, Eun-Kyung;Kim, Taek-Kyum;Hong, Su-Myeong;Kwon, Hye-Yong;Kwon, Ji-Hyung;Son, Kyung-Ae;Kim, Jang-Eok;Kim, Doo-Ho
    • The Korean Journal of Pesticide Science
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    • v.17 no.4
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    • pp.264-270
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    • 2013
  • Imidacloprid is a systemic insecticide which act as an insect neurotoxin. It used for control of pest such as aphids and other sucking insects in fruits and vegetables. Systemic pesticides move inside a crop following absorption by the plant, and these were converted into a variety of metabolites. Sometimes these metabolites make a problem about safety of agricultural products. So a simultaneous determination method of pesticide and its metabolites is needed, to monitor their presence in agricultural product and study on the fate of pesticide in a plant. This study's aim is to investigate simultaneous analysis method of imidacloprid and its metabolites, imidacloprid guanidine, imidacloprid olefin, imidacloprid urea, and 6-chloronicotinic acid in red pepper using QuEChERS method and LC-MS/MS systems. QuEChERS method was modifed beacuase $MgSO_4$ salts decreased the recoveries of 6-chloronicotinic acid in extraction procedure. Imidacloprid and its metabolites were extracted by acetonitrile with 1% glacial acetic acid and the extracts were purified through QuEChERS with primary secondary amine (PSA) and $C_{18}$ and analyzed with LC-MS/MS in ESI positive mode. Standard calibration curves were made by matrix matched standards and their correlation coefficients were higher than 0.999. Recovery studies were carried out on spiked pepper blank sample at four concentration levels (0.01, 0.04 and 0.1, 0.4 mg/kg). The average recoveries of imidacloprid and its metabolites were in the range of 70~120% with < 20% RSD. This result indicated that the method using QuEChERS and LC-MS/MS was suitable for the simultaneous determination of imidacloprid and its metabolites in red pepper.

Method Development for Determination of Multi-Mycotoxins in Chicken Liver and Kidney Tissues by LC-MS/MS (LC-MS/MS를 이용한 닭 간과 신장 중 곰팡이 독소 6종 동시분석법 개발)

  • Kim, Soohee;Kim, Kwang-Nam;Kim, Hyobi;Song, Jae-Young;Park, Sung-Won
    • Korean Journal of Poultry Science
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    • v.43 no.2
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    • pp.111-118
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    • 2016
  • Mycotoxins are secondary metabolites produced by molds, such as Aspergillus, Fusarium and Penicillium, that have adverse effects on animals and humans. Aflatoxin, ochratoxin, zearalenone, fumonisin and deoxynivalenol are the mycotoxins of greatest agro-economic importance and cause acute disease called mycotoxicoses. Mycotoxicosis in poultry birds results in decreased meat/egg production, immunosuppressant, and hepatotoxicosis. Some of toxins or their metabolites may be retained in animal or human tissues and induce health problems. This study was designed to develop a sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the simultaneous detection and quantification of mycotoxins, such as aflatoxin $B_1$, aflatoxin $M_1$, ochratoxin A, zearalenone, fumonisin B and deoxynivalenol, in chicken liver and kidney tissues. The mycotoxins were extracted and purified using modified QUECHERS methods, separated by LC and detected by an electrospray ionisation interface (ESI) and tandem MS. Good precision and linearity were observed for most of six mycotoxins. The recovery test for each mycotoxin in liver and kidney tissues mostly indicated good average recovery rates between 80.94% and 98.10% and the coefficient of variation mostly under 13.78%, except for aflatoxin $M_1$ and fumonisin $B_1$. The limit of detection (LOD) for six mycotoxins was $7.6{\sim}145.79{\mu}g/kg$ in liver tissues and $6.07{\sim}197.20{\mu}g/kg$ in kidney tissues. The quantification limits (LOQ) for 6 mycotoxins were in the range $23.04{\sim}441.78{\mu}g/kg$ in liver tissues and $18.40{\sim}597.59{\mu}g/kg$ in kidney tissues, respectively. The developed multi-mycotoxin method in this study permits simultaneous, simple, and rapid determination of several co-existing mycotoxins in chicken liver and kidney tissues.

Component Analysis of Suaeda asparagoides Extracts (나문재 추출물의 성분 분석)

  • Yang, Hee-Jung;Park, Soo-Nam
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.34 no.3
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    • pp.157-165
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    • 2008
  • In the previous study, the anti-oxidant activity of oxtract/fraction of Sueada aspparagoides(SA) and the stability test for the cream containing SA extract were investigated respectively[1,2]. In this study, the components of SA extract were analyzed by TLC, HPLC, and LC/ESI-MS/MS, $^1H$-NMR. TLC chromatogram of ethyl acetate fraction of SA extract revealed 5 bands $(SA1{\sim}SA5)$. HPLC chromatogram of aglycone fractions obtained from deglycoylation reaction of ethyl acetate fraction showed 2 bands (SAA 2 and SAA 1), which were identified as quercetin (composition ratio, 16.88%) and kaempferol (83.12%) in the order of elution time. Among 5 bands of TLC chromatogram, 4 bands $(SA2{\sim}SA5)$ also were Identified as kaempferol-3-O-glucoside (SA 2), quercetin-3-O-glucoside (SA3), kaempferol-3-O-rutinoside (SA 4), quercetin-3-O-rutinoside (SA 5) by LC/ESI-MS/MSMS/MS. respectively. The spectrum generated for SAA 1 by LC/ESI-MS/MS in the negative ion mode also gave the ion corresponding to the deprotonated aglycone $[M-H]^-$ (285m/z), the $^1H$-NMR spectrum contained signals [${\delta}$ 6.19 (1H, d, J=1.8Hz, H-6), ${\delta}$ 6.44 (1H, d, J=1.8Hz, H-8), ${\delta}$ 6.92 (2H, d, J=9.0Hz, H-3', 5'), ${\delta}$ 8.04 (2H, d, J=9.0Hz, H-2', 6', thus SAA 1 was identified as kaempferol. SAA 2 yielded the deprotonated agycone ion $[M-H]^-$ (301m/z), $^1H$-NMR spectrum showed signals [${\delta}$ 6.20 (1H, d, J=2.0Hz, H-6), ${\delta}$ 6.42 (1H, d, J=2.0Hz, H-8), ${\delta}$ 6.90 (1H, d, J=8.6Hz, H-5'), ${\delta}$ 7.55 (1H, dd, J=8.6, 2.2Hz, H-6'), ${\delta}$ 7.69 (1H, d, J=2.2Hz, H-2', thus SAA 2 was Identified as quercetin. In conclusion, with the anti-oxidant activity and the stability test reported previously, component analysis of SA extracts could be applicable to new cosmeceuticals.

Optimization of the Flip Angle and Scan Timing in Hepatobiliary Phase Imaging Using T1-Weighted, CAIPIRINHA GRE Imaging

  • Kim, Jeongjae;Kim, Bong Soo;Lee, Jeong Sub;Woo, Seung Tae;Choi, Guk Myung;Kim, Seung Hyoung;Lee, Ho Kyu;Lee, Mu Sook;Lee, Kyung Ryeol;Park, Joon Hyuk
    • Investigative Magnetic Resonance Imaging
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    • v.22 no.1
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    • pp.1-9
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    • 2018
  • Purpose: This study was designed to optimize the flip angle (FA) and scan timing of the hepatobiliary phase (HBP) using the 3D T1-weighted, gradient-echo (GRE) imaging with controlled aliasing in parallel imaging results in higher acceleration (CAIPIRINHA) technique on gadoxetic acid-enhanced 3T liver MR imaging. Materials and Methods: Sixty-two patients who underwent gadoxetic acid-enhanced 3T liver MR imaging were included in this study. Four 3D T1-weighted GRE imaging studies using the CAIPIRINHA technique and FAs of $9^{\circ}$ and $13^{\circ}$ were acquired during HBP at 15 and 20 min after intravenous injection of gadoxetic acid. Two abdominal radiologists, who were blinded to the FA and the timing of image acquisition, assessed the sharpness of liver edge, hepatic vessel clarity, lesion conspicuity, artifact severity, and overall image quality using a five-point scale. Quantitative analysis was performed by another radiologist to estimate the relative liver enhancement (RLE) and the signal-to-noise ratio (SNR). Statistical analyses were performed using the Wilcoxon signed rank test and one-way analysis of variance. Results: The scores of the HBP with an FA of $13^{\circ}$ during the same delayed time were significantly higher than those of the HBP with an FA of $9^{\circ}$ in all the assessment items (P < 0.01). In terms of the delay time, images at the same FA obtained with a 20-min-HBP showed better quality than those obtained with a 15-min-HBP. There was no significant difference in qualitative scores between the 20-min-HBP and the 15-min-HBP images in the non-liver cirrhosis (LC) group except for the hepatic vessel clarity score with $9^{\circ}$ FA. In the quantitative analysis, a statistically significant difference was found in the degree of RLE in the four HBP images (P = 0.012). However, in the subgroup analysis, no significant difference in RLE was found in the four HBP images in either the LC or the non-LC groups. The SNR did not differ significantly in the four HBP images. In the subgroup analysis, 20-min-HBP imaging with a $13^{\circ}$ FA showed the highest SNR value in the LC-group, whereas 15-min-HBP imaging with a $13^{\circ}$ FA showed the best value of SNR in the non-LC group. Conclusion: The use of a moderately high FA improves the image quality and lesion conspicuity on 3D, T1-weighted GRE imaging using the CAIPIRINHA technique on gadoxetic acid, 3T liver MR imaging. In patients with normal liver function, the 15-min-HBP with a $13^{\circ}$ FA represents a feasible option without a significant decrease in image quality.