固相萃取-液相色谱串联质谱法测定葡萄酒中27种农药残留

Determination of Residual Amounts of 27 Pesticides in Grape Wine with SPE pretreatment(LC-MS/MS)

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.