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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.
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Yujin Lim,Aelim Kim,Yong-Moon Lee,Hwangeui Cho 한국분석과학회 2023 분석과학 Vol.36 No.6
Zidovudine is an antiretroviral agent prescribed for the prevention and treatment of human immunodeficiency virus/acquired immune deficiency syndrome (HIV/AIDS). It is typically recommended to be used in combination with other antiretroviral drugs. Zidovudine has the potential to generate Nnitrosodimethylamine (NDMA) in the presence of dimethylamine and nitrite salt under acidic reaction conditions during the drug manufacturing process. NDMA is a potent human carcinogen that may be detected in drug substances or drug products. An analytical method was developed to determine NDMA in pharmaceuticals including zidovudine using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/ MS). The analysis involved reversed-phase chromatography on a Kinetex F5 column with a mobile phase comprising water-acetonitrile mixtures. The detection of positively charged ions was conducted using atmospheric pressure chemical ionization (APCI). The calibration curve demonstrated excellent linearity (r = 0.9997) across the range of 150 ng/mL with a highly sensitive limit of detection (LOD) at 0.3 ng/mL. The developed method underwent thorough validation for specificity, linearity, accuracy, precision, robustness, and system suitability. This sensitive and specific analytical method was applied for detecting NDMA in zidovudine drug substance and its formulation currently available in the market, indicating its suitability for drug quality management purposes.
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GC-MS/MS를 이용한 원유 원료 중 농약 동시분석법 확립
최영내,신윤호,조황의,김정복,Young Nae Choi,Yoon ho Shin,Hwangeui Cho,Jung Bok Kim 한국식품위생안전성학회 2023 한국식품위생안전성학회지 Vol.38 No.6
본 연구에 선정된 농약성분은 사용목적에 따른 분류 기준으로 살충제에 해당되며, 유효성분 조성에 따른 분류의 경우 유기인계 농약성분 2가지, 농약 중 가장 범용적으로 사용되고 있는 피레스로이드 농약성분 3가지이다. 원유 중 5가지 농약성분인 chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin 및 permethrin 등은 시료와 분석물질의 특성을 고려하여 2그룹으로 나누어 시료전처리를 확립하였고 LLE와 카트리지를 이용하여 원유 중에 농약성분을 분석하였다. GC-MS/MS을 이용하였고 사용된 컬럼은 HP-5MS(30 m×0.25 mm ID, 0.25 ㎛)를 사용하였다. 검량선의 농도는 10-200 ng/mL이고, 각각의 분석물질의 결정계수(R<sup>2</sup>)가 0.997 이상으로 확인하였다. 정밀성과 정확성을 확인하기 위해 검량선 내 3가지 농도 선정하여 일내와 일간의 정밀성 및 정확성을 측정하였다. 5개의 분석물질의 일내 일간 정밀성은 10.3% 이하, 정확성은 100.9-117.5%의 범위로 확인되었다. 확립된 분석법의 회수율 측정을 위해 농약기준 규격의 잔류허용기준을 참고하여 가장 낮은 농도를 선정하였고 회수율은 86.1%-102.1%로 확인되었다. 물질의 검출한계 및 정량한계의 농도 범위는 37.5-125 ng/mL로 산출되었다. 측정 불확도를 산출하기 위해 설정된 불확도 요인을 설정하여 산출하였다. 그 결과 신뢰수준 95% k=2에서 chlorpyrifos 6.35±0.32 mg/kg, chlorpyrifos-methyl 6.20±0.17 mg/kg, cypermethrin 6.45±0.45 mg/kg, deltamethrin 6.28±0.20 mg/kg, permethrin 6.10±0.56 mg/kg 으로 불확도 값을 산출하여 원유 중 5가지 농약 성분의 유효성이 검증된 분석법을 확립하였다. 본 연구결과를 통해 원유 중 미량으로 잔류할 수 있는 농약성분의 검출이 가능한 것으로 나타났다. 본 연구결과는 기준규격 설정과 관리에 좋은 참고 자료가 될 것으로 판단된다. GC-MS/MS using liquid-liquid extraction (LLE) and C18 cartridges was used to identify and quantify levels of chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin and permethrin in bulk raw milk. A calibration curve spanning 10 ng/mL to 200 ng/mL was obtained with a satisfactory correlation coefficient of 0.99. The limits of detection (LOD) and limits of quantitation (LOQ) for chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin, and permethrin in the matrix ranged from 0.06 to 1.81 ng/mL and 0.19 to 6.04 ng/mL, respectively. The recoveries of 5 pesticides from spiked samples at 37.5-125 ng/mL ranged from 86.1 to 102.1%. The measurement of uncertainty of the GC-MS/MS method for these five pesticides was developed based on the analytical process and quantification. An analysis method that is easier and faster than the method specified in the Korean food standards codes for analyzing these five pesticides in raw material milk was developed. Moreover, the analytical method for chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin, and permethrin in bulk raw milk by GC-MS/MS was established.
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