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액체크로마토그래피-질량분석기를 이용한 쌀 중 스테리그마토시스틴과 아플라톡신 시험법 개발
이봄내 ( Bom Nae Lee ),권진욱 ( Jin-wook Kwon ),정은아 ( Eun A Chong ),천소영 ( So Young Chun ),강길진 ( Gil Jin Kang ) 한국환경농학회 2019 한국환경농학회 학술대회집 Vol.2019 No.-
Sterigmatocystin is a mycotoxin produced by fungi of the genus Aspergillus (mainly A. nidulans and A versicolor). Sterigmatocystin shares its biosynthetic pathway with aflatoixns. The aim of this study is to optimize the liquid chromatography-tandem mass spectrometry method for determination of sterigmatocystin and aflatoxins (B<sub>1</sub>,B<sub>2</sub>,G<sub>1</sub>,G<sub>2</sub>)inrice, simultaneously. Targetsampleswereextractedwith0.1 % formic acid in 50 % acetonitrile then purified with Isolute cartridge (solid phase extraction). Separations by HPLC were mainly conducted with a Cadenza C18 analytical column using 0.1% formic acid and 5 mM ammonium formate under gradient condition with ultrapure water and methanol. The mycotoxins were detected by electrospray ionization in positive or negative ion with multiple reaction monitoring (MRM) and mass spectrometric conditions were optimized in order to increase selectivity and sensitivity. The developed method was validated in terms of linearity, trueness, precision, limits of detection and quantification. Matrix-matched calibration was used for quantification, with regression coefficients (R2) ≥ 0.98.
신용운 ( Yong Woon Shin ),신춘식 ( Choonshik Shin ),이지은 ( Ji-eun Lee ),서수진 ( Sujin Seo ),권진욱 ( Jin-wook Kwon ),강길진 ( Gil-jin Kang ) 한국환경농학회 2019 한국환경농학회 학술대회집 Vol.2019 No.-
Polybrominated biphenyls (PBBs) are a class of brominated hydrocarbons with 209 possible compounds, referred to as PBB congeners. PBBs are lipophilic compounds with a low vapour pressure and low water solubility which decreases with increasing degree of bromination and chemically stable, persistent in the environment and bioaccumulative. Especially, hexabrominated bipheyls (HBBs) of PBBs are most widely used for plasticizers and flame retardants were designated as persistent organic pollutants (POPs) by Stockholm Convention in 2009. As a part of the food safety management of POPs, six PBBs which are mainly concerned and prioritized to investigate, were monitored from domestically distributed fisheries and animal products in Korea. Gas liquid chromatography-high resolution mass spectrometry was used with selected ion monitoring and stable isotope dilution method (GC-HRMS-SIM) for qualification and quantitation. LODs and LOQs were set at the levels of 3 pg/g and 10 pg/g on the wet weight basis, respectively. Frequencies of occurrence of PBBs from the 154 foods; 77 fisheries and 77 animal products, were 6.7 % in fisheries, and 2.4 %, respectively in animal product with detection of different congeners below or at the levels of LOQs.
농산물 중 Isofetamid와 대사체의 분석법 검증 및 측정불확도 추정
김지영 ( Ji Young Kim ),최윤주 ( Youn Ju Choi ),송지영 ( Ji Young Song ),한아름 ( 아름 Han ),도정아 ( Jung Ah Do ),장문익 ( Moon Ik Chang ),이규식 ( Gyu Seek Rhee ),강길진 ( Gil Jin Kang ) 한국환경농학회 2016 한국환경농학회 학술대회집 Vol.2016 No.-
Isofetamid is the fungicide belonging to SDHI(Succinate Dehydrogenase Inhibitors) group. It inhibits succinate-dehydrogenase in complex II of fungal respiration. Isofetamid is primarily metabolized by o-dealkylation to the 4HP metabolite with subsequent conjugations leading to its glucose conjugate GPTC. In general, Isofetamid expressed as sum of isofetamid and metabolite GPTC expressed as isofetamid. In this study, validation of analytical method of Isofetamid and its metabolite GPTC was carried out using HPLC/MS-MS and was demonstrated to estimate the measurement uncertainty of Isofetamid and its metabolite. The sources of measurement uncertainty (i.e. sample weight, final volume, standard weight, purity, standard solution, calibration curve, recovery and repeatability) in associated with the analysis of Isofetamid and its metabolite GPTC were evaluated. Prior to measurement of uncertainty, the analytical method was validated for linearity, limit of detection (LOD 0.003 mg/kg), limit of quantification (LOQ 0.01 mg/kg), precision and accuracy (less than RSD of 10 %). The content of fortified Isofetamid and GPTC from agricultural products was estimated at a 95% confidence level. The results of the recovery test were 73.1%-119.9%. These validation results demonstrated that this analytical method could be suitable for the determination of isofetamid and GPTC in agriculural products complying with performance requirements of CODEX guideline.