固相萃取-气相色谱质谱法同时测定水果蔬菜中13种三唑类杀菌剂  

Simultaneous determination of 13 triazole fungicides in fruit and vegetables by solid phase extraction and gas chromatography-mass spectrometry

作　　者：陶凌云[1] 

机构地区：[1]延安市疾病预防控制中心,陕西延安716000

出　　处：《中国卫生检验杂志》2017年第23期3385-3387,3405,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立固相萃取(SPE)-气相色谱质谱法同时测定水果蔬菜中戊菌唑、四氟醚唑、氟菌唑、己唑醇、乙环唑、腈菌唑和粉唑醇等13种三唑类杀菌剂残留量的检测方法。方法采用乙腈、Carbori/NH2固相萃取柱净化提取样品中的待测组分,气相色谱串联质谱法分析,多反应监测模式(MRM)质谱检测,通过外标法定量。结果在优化实验条件下,13种三唑类杀菌剂的回归方程均呈较好的线性关系,相关系数在0.995以上,检出限在0.2μg/L^6.2μg/L,定量限为0.5μg/L^7.9μg/L。在0.5μg/L、1.0μg/L、2.0μg/L 3种添加水平下,该方法的平均回收率在81.31%~104.43%,相对标准偏差(RSD)在2.33%~9.51%。结论该方法背景干扰低,具有操作快捷简单、准确度和灵敏度高等特点,定量限低于有关文献报道及国家标准值。满足同时测定水果中13种三唑类杀菌剂农药残留的检测要求。Objective To develop a method for the simultaneous determination of 13 triazole fungi-cides such as penconazole,tetraconazole,triflumizole,hexazol,ethylozole,hexaconazole,flutriafol in fruits and vegatables by gas chromatography-tandemmass spectrometry（ GC-MS/MS）. Methods The triazole fungicides were extracted from the samples with acetoni-trile and cleaned-up with solid phase extraction（ SPE） on a Carbon/NH2 cartridge. The detection was carried out by GC/MS in the multiple reaction monito-ring（ MRM） mode,and the quantification analysis was performed by external standard method. Results The calibration curves showed good linearity under the optimized conditions. The correlation coefficients were greater than 0. 995. The detection limit was within 0. 2 μg/L-6. 2 μg/L,and the limit of quantification was within 0. 5 μg/L-7. 9 μg/L. The average recoveries of the 13 fungicides spiked in the fruits at the levels of 0. 5 μg/L,1. 0 μg/L and 2. 0 μg/L were within 81. 31%-104. 43%,and the relative standard deviations（ RSDs） were within 2. 33%-9. 51%. Conclusion The method possesses low background,high sensitivity and quantification limits lower than that of the national standard and the values reported in the relevant literature. It can be applied to the routine analysis of the 13 triazole fungicides in fruits.

关 键 词：固相萃取 气相色谱质谱 水果 三唑类杀菌剂 

分 类 号：O657.63[理学—分析化学]