固相萃取–气相色谱–串联质谱法测定甘蓝类蔬菜中氟啶虫酰胺和嘧菌环胺

Determination of fluridinamide and cyprodinil in cabbage vegetables by solid phase extraction–gas chromatography–tandem mass spectrometry

建立固相萃取-气相色谱-串联质谱(GC-MS-MS)测定甘蓝类蔬菜中氟啶虫酰胺和嘧菌环胺残留量的分析方法。甘蓝类蔬菜样品经乙腈提取后,用ENVI-Carb活性炭固相萃取柱净化,乙腈-甲苯(3∶1)溶液进行洗脱,采用GC-MS-MS法测定,以保留时间和选择性反应监测(MRM)离子对定性,色谱峰面积定量。氟啶虫酰胺和嘧菌环胺的质量浓度在0.05~2.0μg/mL范围内与色谱峰面积呈良好的线性关系,线性相关系数均大于0.998,检出限分别为0.005,0.008mg/kg。样品加标回收率为87.4%~97.3%,测定结果的相对标准偏差为1.3%~3.2%(n=6)。该方法灵敏度和准确度高,适用于甘蓝类蔬菜中氟啶虫酰胺和嘧菌环胺残留的测定。

A method for the determination of fluridinamide and cyprodinil in cabbage vegetables by solid phase extraction-gas chromatography-tandem mass spectrometry (GC-MS-MS) was established.The samples of cabbage vegetables were extracted by acetonitrile,extracted solution was purified by ENVI-Carb activated carbon solid phase extraction column,eluted by acetonitrile-toluene (3:1) solution,and determined by GC-MS-MS.Retention time and selective reaction monitoring (MRM) ion pair were determined qualitatively and chromatographic peak area quantitatively determinated.The mass concentration of fluridinamide and cyprodinil had good linear relationship with its chromatographic peak area in the range of 0.05-2.0 μg/mL.The linear correlation coefficients were more than 0.998.The detection limits were 0.005 and 0.008 mg/kg,respectively.The average recoveries of samples were ranged 87.4%-97.3%.The relative standard deviation of the determination results were 1.3%-3.2%(n=6).The method has high sensitivity and accuracy,it is suitable for the detection of fluridinamide and cyprodinil in cabbage vegetables.