分散液液微萃取与GC-MS联用分析葡萄酒中苯醚甲环唑残留

Development and Application of a Screening Method for Difenoconazole Determination in Wine Samples Using DLLME-GCMS

为建立葡萄酒中苯醚甲环唑的测定方法,以超声辅助-凝固-漂浮分散液液微萃取(UADLLME-SFO)为富集、净化手段,采用气相色谱-质谱(GC-MS)联用法检测葡萄酒中苯醚甲环唑的残留量,应用正交试验对萃取参数进行优化。结果表明,最适宜的萃取条件为:萃取剂十一醇30μL、超声时间5 min、氯化钠浓度30 g·L^(-1),此条件下苯醚甲环唑的检出限为2.3 ng·L^(-1),相对标准偏差(n=5)在3.5%~6.2%之间,当添加浓度为1μg·L^(-1)和50μg·L^(-1)时,苯醚甲环唑的添加回收率在90.2%~98.4%之间。本研究结果为葡萄酒中苯醚甲环唑残留的检测提供了研究方法和科学依据。

In order to the determin the difenoconazole content in wine, a method using ultrasound assisted dispersive liquid-liquid microextraction on solidification of floating organic droplets （UA-DLLME-SFO） coupled to gas chromatography mass spectrometry （GC-MS） was developed. The key extraction parameters influencing extraction efficiencies were investigated and optimized by orthogonal experiments. The results showed that, the optimized conditions were as follows ： 30 μL 1 - undecanol was used, ultrasonic time was 5 min and concentration of NaCl was 30 g. L-1 Under the optimized conditions, the detection limits obtained for difenoconazole was 2.3 ng.L-1. The relative standard deviations were 3.5% to 6.2% （n = 5）. The recoveries of difenoconazole was in the range of 90.2% to 98.4% at spiked levels of 1 μg.L-1and 50 μg.L-1. This study provides a method for the analysis and evaluations of difenoconazole in wine.