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흑염소에서의 철쭉으로부터 유래된 그레이아노톡신 중독증 증례
김지현 ( Ji-hyeon Kim ),정지열 ( Ji-youl Jung ),최은진 ( Eunjin Choi ),신은경 ( Eunkyung Shin ),정지연 ( Jiyeon Jeong ),이경현 ( Kyunghyun Lee ),김선춘 ( Suncheun Kim ),소병재 ( Byungjae So ) 한국가축위생학회 2017 韓國家畜衛生學會誌 Vol.40 No.4
A 3 year-old black goat was presented to Animal and Plant Quarantine agency for diagnosis in June, 2017. She was intaken feed with Rhododendron schlippenbachii the day before death. The clinical signs included loss of appetite, lethargy, hypersalivation, astasia, yelling. At necropsy, foamy discharge were observed in the airway. Histologically, foreign body, eosinphil and macrophges was observed in alveolar lumen of lung. Grayanotoxin derived from Rhododendrons was detected in ruminal contents. Based on the pathological and toxine examination, we diagnosed this case as grayanotoxin poisoning in a black goat.
Cho, Byungsuk,Kim, Suncheun,In, Sangwhan,Choe, Sanggil Elsevier 2017 Forensic Science International Vol.278 No.-
<P><B>Abstract</B></P> <P>A liquid chromatography–tandem mass spectrometry method with solid-phase extraction (SPE) was developed and validated for the detection and quantitation of bentazone and its two hydroxylated metabolites, 6-hydroxybentazone and 8-hydroxybentazone, in postmortem blood. Sample cleanup was performed using a hydrophilic-lipophilic balanced (HLB) SPE cartridge and then separated on a C18 LC column using a gradient elution of 0.1% formic acid in distilled water and 0.1% formic acid in methanol. The identification of bentazone and its hydroxylated metabolites was performed using tandem mass spectrometry with electrospray ionization in negative ion mode with selective reaction monitoring. The retention times of bentazone, 6-hydroxybentazone, 8-hydroxybentazone, and 2-methyl-4-chlorophenoxyacetic acid (MCPA, internal standard) appeared separately in the chromatogram. The matrix effect, recovery, and process efficiency of bentazone were 75.3%, 103.6% and 77.9%, respectively. In addition, good accuracy (88.2–110.5%), precision (0.5–7.5%, bias), and linearity (5–500ng/mL) were obtained with this method. The limit of detection (LOD) of bentazone, 6-hydroxybentazone, and 8-hydroxybentazone were 0.05, 0.5, and 0.5ng/mL, respectively. The method developed herein was applied to authentic samples from three fatal cases from 2016 for the determination of the corresponding bentazone and its metabolites levels. The concentration ranges of bentazone, 6-hydroxybentazone, and 8-hydroxybentazone in the heart blood from the three victims were 46.0–91.8, 4.2–6.2, and 0.2–0.6μg/mL, respectively.</P> <P><B>Highlights</B></P> <P> <UL> <LI> A LC–MS/MS method was developed to determine bentazone concentrations in blood specimens. </LI> <LI> Target analytes were bentazone and its two hydroxylated metabolites. </LI> <LI> The solid phase extraction of bentazone and its metabolites from blood was used. </LI> <LI> The method was selective and sensitive for each analyte. </LI> <LI> Fatal cases of bentazone poisoning by oral ingestion were applied. </LI> </UL> </P>
Su Youn Ahn,Suncheun Kim,Hwangeui Cho 한국분석과학회 2022 분석과학 Vol.35 No.2
Grayanotoxin-contaminated honey exhibits toxicity. In this study, a reliable and sensitive liquidchromatography– tandem-mass-spectrometric method (LC–MS/MS) was developed and validated for the quantitation of grayanotoxin I and grayanotoxin III in honey. The grayanotoxins were extracted from honey via solid phase extraction and separated on a biphenyl column with a mobile phase consisting of 0.5 % acetic acid in water and methanol. Mass spectrometric detection was performed in the multiple-reaction monitoring mode with positive electrospray ionization. The calibration curve covered the range 0.25 to 100 μg/g. The intra- and interday deviations were less than 10.6 %, and the accuracy was between 94.3 and 114.0 %. The validated method was successfully applied to the determination of grayanotoxins in mad honey from Nepal. The concentrations of grayanotoxin I and grayanotoxin III in 33 out of 60 mad honey samples were 0.75 – 64.86 μg/g and 0.25 – 63.99 μg/g, respectively. The method established herein would help in preventing and confirming grayanotoxin poisoning.
Hong, Ran Seon,Cho, Hwang Eui,Kim, Dong Woo,Woo, Sang Hee,Choe, Sanggil,Kim, Suncheun,Hong, Jin Tae,Moon, Dong Cheul Korean Magnetic Resonance Society 2013 Journal of the Korean Magnetic Resonance Society Vol.17 No.1
For a case study of suspected paraquat intoxication, we developed a simple and rapid method of $^1H$ qNMR to determine the mili-molar amount of paraquat in postmortem blood samples. There were no interfering signals from endogenous compounds in the chemical shift of paraquat and diquat (internal standard). The amount of sample used ranged from 0.25 mM to 10.0 mM. Diquat, which has similar physicochemical properties with paraquat, was chosen as an internal standard. The NMR experimental conditions, relaxation delay time and CPMG spin-echo pulse sequence were optimized. The developed method was validated in terms of specificity, accuracy, precision, matrix effect, recovery, limit of detection (LOD), and low limit of quantification (LLOQ). The proposed qNMR method provided a simple and rapid assay for the identification and quantification of the quaternary ammonium herbicide, "paraquat" in postmortem blood samples. This method was tested by using the blood from the heart of a man who was intoxicated with paraquat. In this particular case, the level of paraquat was 1.07 mM in the blood. For the determination of quaternary ammonium herbicides, qNMR could also be used to provide a better understanding of the currently available techniques.
Survey of ERETIC2 NMR for quantification
Hong, Ran Seon,Hwang, Kyung Hwa,Kim, Suncheun,Cho, Hwang Eui,Lee, Hun Joo,Hong, Jin Tae,Moon, Dong Cheul Korean Magnetic Resonance Society 2013 Journal of the Korean Magnetic Resonance Society Vol.17 No.2
The ERETIC (Electronic REference To access In vivo Concentrations)2 method is a new qNMR experimental technique to measure analytes based on the signal of the reference compound without additional hardware equipment. In this study, ERETIC2 method was validated, and we sought to identify whether it would be possible to apply this method to a specific compound analysis of metabolites in plant. The $90^{\circ}$ pulse value (P1) and spin-lattice relaxation time ($T_1$) of each compound were measured for ERETIC2. The $9^1H$ of 3-(trimethylsilyl) propionic-2,2,3,3-$d_4$ acid (TSP) was used as a reference peak for ERETIC 2, and then, a suitable solvent and pulse sequence for each compound were selected. Under the NOESY-presat sequence, the relative accuracy error for quantitative analyses of primary metabolites was within the range of 5%, with the exception of glucose, which showed ${\geq}$ 55% error due to saturation. It showed excellent results for the quantification of glucose by using a $30^{\circ}$ pulse sequence, which did not suppress the water peak. In addition, the quantitative accuracy for secondary metabolites was extremely accurate, with an error ${\leq}$5% when considering the purity of the standard sample. The ERETIC2 method showed outstanding linearity, precision, and accuracy.