QuEChERS-气相色谱–串联质谱法测定海南淡水鱼中有机氯农药残留

Determination of organochlorine pesticide residues in Hainan freshwater fishes by QuEChERS combined with gas chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  二氧化锆  气相色谱-串联质谱法  有机氯  淡水鱼

英文关键词:QuEChERS  zirconium dioxide  gas chromatography-tandem mass spectrometry  organochlorine pesticides  freshwater fishes

中文摘要:

      目的 建立QuEChERS结合气相色谱－串联质谱(gas chromatography-tandem mass spectrometry, GC-MS/MS)检测鱼肉中12种有机氯农药(organochlorine pesticides, OCPs)残留的快速检测方法。方法 样品采用丙酮+正己烷(1:1, V:V)超声提取, 经0.4 g PSA、0.4 g C18、1.2 g无水硫酸镁和40 mg二氧化锆净化, 采用GC-MS/MS检测。结果 样品在1.6~40 ng/mL范围内线性良好, r2≥0.9985; 3个添加水平(n=6)平均回收率为90.8%~121.6%, RSD为1.3%~7.5%; 检出限为0.04~0.72 μg/kg, 定量限为0.13~2.43 μg/kg。结论 该方法灵敏度高、快速、准确, 能够满足鱼肉中多种OCPs的检测要求。

英文摘要:

      Objective To establish a rapid method for determination of 12 organochlorine pesticides (OCPs) residues in the fish by QuEChERS combined with gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The samples were extracted by ultrasonic with acetone and n-hexane (1:1, V:V), purified with 0.4 g PSA, 0.4 g C18, 1.2 g anhydrous magnesium sulfate and 40 mg zirconium dioxide, and detected by GC-MS/MS. Results The linearity was good in the range of 1.6-40 ng/mL, with correlation coefficients all above 0.9985. The recoveries of the 3 additive levels (n=6) were 90.8%-121.6%, and RSDs were 1.3%-7.5%. The limits of detection were 0.04-0.72 μg/kg, and the limits of quantitation were 0.13-2.43 μg/kg. Conclusion The method is sensitive, fast and accurate, which can meet the requirements of OCPs detection in fishes.