改良QuEChERS法结合气相色谱串联质谱测定果蔬中20种杀菌剂

Determination of 20 kinds of fungicide residues in vegetables and fruits by gas chromatography-mass spectrometry combined modified QuEChERS method

中文关键词:  气相色谱/质谱法  QuEChERS  杀菌剂  残留测定

英文关键词:gas chromatography-mass spectrometry  QuEChERS  fungicides  residue detection

中文摘要:

      目的 建立果蔬中20种杀菌剂(三环唑、五氯硝基苯、嘧霉胺、乙烯菌核利、百菌清、三唑酮、戊菌唑、腐霉利、三唑醇、多效唑、稻瘟灵、抑霉唑、咯菌腈、氟硅唑、腈菌唑、肟菌酯、丙环唑、咪鲜胺、腈苯唑、苯醚甲环唑)残留量的QuEChERS-GC/MS快速测定方法。方法 以生菜、毛瓜、葡萄、李子为原料, 样品经乙腈提取, PSA粉50.0 mg、Al2O3粉50.0 mg和NH2粉30.0 mg除杂净化后, 用GC/MS外标法定量。结果 三环唑等20种杀菌剂在0.025~0.250 mg/L的质量浓度范围内线性关系良好, 相关系数为0.9974~1.0000。添加水平为0.05、0.1、0.2 mg/kg时, 除百菌清外, 其余19种杀菌剂平均回收率范围均处于83%~112%之间, 相对标准偏差(RSD)小于11.0%, 方法的检出限(LOD)为0.2~11.8 μg/kg之间。结论 本方法具有灵敏、快速、简便等特点, 能满足果蔬中三环唑等20种农药杀菌剂的检测要求。

英文摘要:

      Objective To develop a QuEChERS method combined with gas chromatography mass spectrometry (GC/MS) for the determination of 20 kinds of fungicide residues (tricyclazole, quintozene, pyrimethanil, vinclozolin, chlorothalonil, triadimefon, penconazole, procymidone, triadimenol, paclobutrazol, isoprothi-olane, imazalil, fludioxonil, flusilazole, myclobutanil, trifloxystrobin, propiconazol, prochloraz, fenbu-conazole and difenoconazole) in vegetables and fruits. Methods Twenty kinds of fungicides residues were extracted from the samples (lettuce, hairy squash, grape and plum) with acetonitrile, and then detected by GC/MS with external standard method after being cleaned up with three sorbents (PSA 50.0 mg, Al2O3 50.0 mg and NH2 30.0 mg). Results The method showed a good linearity over the range of 0.025~0.250 mg/L with correlation coefficients of 0.9974~1.0000. The recoveries of fungicides, except Chlorothalonil, were in the range of 83%~112% with the spiked levels of 0.05, 0.1 and 0.2 mg/kg into four vegetables and fruits matrixes, and the relative standard deviations (RSDs) were almost not more than 11.0%. The limits of detections (LODs) were in the range of 0.2~11.8 μg/kg, respectively. Conclusion The method is sensitive, rapid and simple, and can be used for the determination of 20 kinds of fungicides residues in vegetables and fruits.