GC-MS/MS法测定草莓中吡唑醚菌酯 残留量及安全评价

本文建立了气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)测定草莓中吡唑醚菌酯的含量, 〖JP+1〗通过探究吡唑醚菌酯在草莓中的残留及消解动态评估吡唑醚菌酯的膳食风险?样品经1.0%甲酸乙腈提取, Cleanert MAS-Q净化管净化, DB-5 MS毛细管气相色谱柱分离, 采用多反应离子监测模式检测?吡唑醚菌酯在质量浓度为0.001~0.200 mg/L范围内线性关系良好( r =0.999 8), 在0.02~2.0 mg/kg添加水平下, 草莓中吡唑醚菌酯的平均回收率为96.8%~101.4%, 相对标准偏差为1.8%~3.3%?定量限为0.020 mg/kg?吡唑醚菌酯在草莓中的残留规律符合一级动力学方程, 其消解半衰期在2.2~3.0 d?膳食风险评估表明末次施药5 d后一般人群吡唑醚菌酯国家估算每日摄入量(the national estimated daily intake, NEDI)为1.34 mg, 占日允许摄入量的70.9%, 我国居民对吡唑醚菌酯长期膳食摄入风险较低, 不会对人体健康产生不可接受的风险?

Residue analysis and safety evaluation of pyraclostrobin in strawberry by GC-MS/MS

A gas chromatography-tandem mass spectrometry (GC-MS/MS) analytical method was established for determination of pyraclostrobin residue in strawberry, and the dietary risk of pyraclostrobin was assessed by exploring the residue and digestion dynamics of pyraclostrobin. Sample was extracted with acetonitrile (acidified with formic acid 1.0%), cleaned up by Cleanert MAS-Q, isolated by the GC system equipped with DB-5 MS UI fused silica capillary column, and detected with electron ionization in a multiple reaction monitoring mode (MRM). The results indicated that pyraclostrobin had a good linear relationship in the range of 0.001-0.200 mg/L ( r =0.999 8). At the three spiking levels from 0.02 to 2.0 mg/kg, the average recoveries of pyraclostrobin in strawberry were in the acceptable ranges of 96.8%-101.4%, with the RSDs of the method ranged from 1.8% to 3.3%. The limit of quantitation was 0.020 mg/kg. The digestion state of pyraclostrobin in strawberry accorded with the first-order degradation kinetics, and the half-life of digestion was 2.2-3.0 d. The national estimated daily intake of pyraclostrobin at fifth day after the last application was 1.34 mg, and the risk probability was 70.9%, indicating that the long-term dietary intake risk of pyraclostrobin would not cause unacceptable risks to human health.