CAJ | 학술논문

建立了固相萃取-气相色谱-质谱(SPE-GC-MS)检测鳗鱼中三氯杀螨醇残留量的分析方法.样品先用正己烷配合乙腈、水均质提取,再加入氯化钠继续均质,离心分层;取部分乙腈层溶液浓缩后过Florisil柱净化,用正己烷淋洗去除油脂,再用乙酸乙酯-正己烷(1∶19, v/v)洗脱分析物;将洗脱液吹干后用正己烷溶解定容,并进行GC-MS分析.采用选择离子监测(SIM)模式检测,外标法定量.在优化的样品前处理条件和GC-MS条件下,方法的定量限(S/N=10)小于0.01 mg/kg;在加标水平为0.01～0.1 mg/kg 时,回收率为91% ～105% ,相对标准偏差为4.3% ～6.1% .该方法准确、灵敏、快速,可满足鳗鱼中三氯杀螨醇残留的检测要求.
건립료고상췌취-기상색보-질보(SPE-GC-MS)검측만어중삼록살만순잔류량적분석방법.양품선용정기완배합을정、수균질제취,재가입록화납계속균질,리심분층;취부분을정층용액농축후과Florisil주정화,용정기완림세거제유지,재용을산을지-정기완(1∶19, v/v)세탈분석물;장세탈액취간후용정기완용해정용,병진행GC-MS분석.채용선택리자감측(SIM)모식검측,외표법정량.재우화적양품전처리조건화GC-MS조건하,방법적정량한(S/N=10)소우0.01 mg/kg;재가표수평위0.01～0.1 mg/kg 시,회수솔위91% ～105% ,상대표준편차위4.3% ～6.1% .해방법준학、령민、쾌속,가만족만어중삼록살만순잔류적검측요구.
A method was developed and applied to determine the residual dicofol in eel by gas chromatography-mass spectrometry (GC-MS). The residue was extracted from homogenized tissue with acetonitrile-water assisted by n-hexane, separated with liquid-liquid partition. A part of the supernatant was purified using solid phase extraction (Florisil column) prior to the GC-MS analysis. The determination was performed in selected ion monitoring (SIM) mode with the external calibration for quantitative analysis. Under the optimized conditions, the quantification limit of the method (S/N=10) was lower than 0.01 mg/kg. The recovery of the method for the spiked standard at the concentration of 0.01-0.1 mg/kg was 91% -105% with the relative standard deviation (RSD) of 4.3% -6.1% . The method is easy, fast, and more sensitive. The method can meet the requirement of the determination of dicofol in eel.