CAJ | 학술논문

建立固相萃取-液相色谱串联质谱的分析方法同时检测葡萄酒中27种农药残留.葡萄酒样品经乙腈超声提取,进行40℃旋转蒸发后,使用CARB/PSA双层SPE小柱进行净化,采用C18色谱柱分离,以含甲酸的乙酸铵缓冲液和乙腈为流动相进行梯度洗脱,在质谱的正离子多反应监测(MRM)模式下进行检测.结果表明:该方法对空白葡萄酒加标水平下27种农药残留的测定线性良好,检测下限(10S/N)在2.5~10μg·kg-1之间,分别在不同3个浓度水平上用标准加入法进行回收试验,平均回收率在60~88%之间,相对标准偏差(n=6)在5.5到16.2%之间.该方法快速准确,灵敏度好,可满足葡萄酒产品的日常检测.
건립고상췌취-액상색보천련질보적분석방법동시검측포도주중27충농약잔류.포도주양품경을정초성제취,진행40℃선전증발후,사용CARB/PSA쌍층SPE소주진행정화,채용C18색보주분리,이함갑산적을산안완충액화을정위류동상진행제도세탈,재질보적정리자다반응감측(MRM)모식하진행검측.결과표명:해방법대공백포도주가표수평하27충농약잔류적측정선성량호,검측하한(10S/N)재2.5~10μg·kg-1지간,분별재불동3개농도수평상용표준가입법진행회수시험,평균회수솔재60~88%지간,상대표준편차(n=6)재5.5도16.2%지간.해방법쾌속준학,령민도호,가만족포도주산품적일상검측.
The method of LC-MS/MS with SPE was applied to the determination of residue amounts of 27 pesticides in grape wine . The grape wine sample was ultrasonic extracted with acetonitrile ,after evaporation to dryness at 40℃ in a rotary evaporator ,The solution was purified on the Carb/PSA double layer SPE column. and the solution was used for LC-MS/MS analysis. The eluate was separated by using C18 column,by using mixtures of ammonium acetate and acetonitrile(contain?ing formic acid)with different ratios as mobiles phase in gradient ,and ESI+and MRM were adopted in MS/MS determina?tion. The linearity of this determination of 27 pesticides residue is well,which using standard addition method in blank grape wine. The detection limits(10S/N)were ranged from 2.5 to 10μg·kg-1 ,and the mean values of recovery in 3 levels found by standard addition method were 60~88%,the RSD(n=6)were in the range of 5.5 to 16.2 . The method is effec?tive,fast and high sensitivity ,meet the request of detection .