摘要
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。
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 (containing formic acid) with different ratios as mobiles phase in gradient , and ESI + and MRM were adopted in MS/MS determination. 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 10 μg. 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.
出处
《福建分析测试》
CAS
2015年第6期7-13,共7页
Fujian Analysis & Testing
基金
福建出入境检验检疫局科技计划项目(FK2011-16)