CAJ | 학술논문

运用简易、高效的QuEChERS前处理方法，建立气相色谱－质谱/质谱联用法（GC－QqQ－MS/MS）检测葡萄酒中4种杀菌剂残留的分析方法．对影响前处理效果的因素进行优化，QuEChERS方法：称取10．0 g样品，加入10．0 mL乙腈，混匀1 min，4℃条件下5000 r/min离心5 min；取上清液10 mL，加入4．0 g无水硫酸镁、1．0 g氯化钠、1．37 g柠檬酸三钠、0．13 g柠檬酸，混匀1 min，4℃条件下5000 r/min离心5 min；取上清液8．0 mL，加入200 mg PSA和1200 mg无水硫酸镁，混匀1 min，4℃条件下10000 r/min离心5 min；取上清液5．0 mL，加入50μL 5％的甲酸/乙腈溶液混匀，氮气吹至近干，正己烷定容至1．0 mL，供GC－MS/MS分析．优化条件下，四种农药在0．01－6 mg/kg之间呈良好线性关系，相关系数r大于0．999，该方法的最低检出限（LOD）在0．0063－0．02 mg/kg之间．该方法简便、快速、灵敏、有机溶剂用量少，适用于葡萄酒中杀菌剂的同时分析．
운용간역、고효적QuEChERS전처리방법，건립기상색보－질보/질보련용법（GC－QqQ－MS/MS）검측포도주중4충살균제잔류적분석방법．대영향전처리효과적인소진행우화，QuEChERS방법：칭취10．0 g양품，가입10．0 mL을정，혼균1 min，4℃조건하5000 r/min리심5 min；취상청액10 mL，가입4．0 g무수류산미、1．0 g록화납、1．37 g저몽산삼납、0．13 g저몽산，혼균1 min，4℃조건하5000 r/min리심5 min；취상청액8．0 mL，가입200 mg PSA화1200 mg무수류산미，혼균1 min，4℃조건하10000 r/min리심5 min；취상청액5．0 mL，가입50μL 5％적갑산/을정용액혼균，담기취지근간，정기완정용지1．0 mL，공GC－MS/MS분석．우화조건하，사충농약재0．01－6 mg/kg지간정량호선성관계，상관계수r대우0．999，해방법적최저검출한（LOD）재0．0063－0．02 mg/kg지간．해방법간편、쾌속、령민、유궤용제용량소，괄용우포도주중살균제적동시분석．
QuEChERS is simple, efficient processing method, Combined this method with a gas chromatography -mass spectrometry /mass spectrometry (GC-QqQ-MS/MS),a method of determination of 4 Fungicides residue in wines is developed.The QuEChERS method:10.0g samples,with 10 mL acetonitrile,mixed 1 min,5000 r/min centrifuge for 5 min under 4 ℃;the supernatant 10mL,add 4 g anhydrous magnesium,1 g sodium chloride,1 .37 g three citric acid,0.13 g citric acid sodium,mixing for 1 min,5000 r/min centrifuge for 5 min under 4 ℃;8 mL supernatant,adding 200 mg PSA and 1200 mg anhydrous magnesium,mixing for 1 min, 10000 r/min centrifugation 5 min under 4 ℃;the supernatant 5 mL,50 μL 5%formic acid /acetonitrile solution blending,nitrogen blowing to nearly dry,n -hexane for 1 mL for GC -MS/MS analysis.Under the optimum conditions,four kinds of fungicides showed a good linear relationship between the 0.01 -6 mg/kg,,correlation coefficient is greater than 0.999.The minimum detection limits of the method (LODs)are in the 0.0063 -0.02 mg/kg.The method is simple, rapid, sensitive, less consume of organic solvent,and is suitable for the simultaneous analysis of fungicides in wine.