超高效液相色谱-串联质谱法同时测定梨中22种农药残留

Simultaneous determination of 22 kinds of pesticide residues in pear by ultra-high performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  梨  同时测定  农药残留

英文关键词:ultra-high performance liquid chromatography-tandem mass spectrometry  pear  simultaneous determination  pesticides residue

中文摘要:

      目的 建立一种超高效液相色谱-串联质谱法测定梨中苯酰菌胺、吡蚜酮、氟虫脲等22种农药残留的分析方法。方法 样品经过高速匀浆后加入乙腈进行提取, 采用ReproSil 100 C18柱(150 mm×2.1 mm, 5 μm), 流速为0.3 mL/min, 柱温为35 ℃进行分离, 应用超高效液相色谱-串联质谱正离子模式下的多反应监测(multiple reaction monitoring, MRM)扫描进行定性定量分析。结果 在浓度测定范围0.010~0.20 mg/L内, 22种农药均成线性关系, 相关系数(r2)为0.9709~0.9998。在0.010、0.050、0.10 mg/kg 3个添加水平下, 22种化合物的回收率为71.4%~106.7%, 相对标准偏差为0.7%~9.9%; 检出限为0.90~4.6 μg/kg, 方法定量限3.0~15.4 μg/kg。在实际梨样品检测到5种农药残留。结论 此方法简便快速、准确度高, 可用于梨样品中22种农药残留的测定。

英文摘要:

      Objective To develop an analytical method based on ultra-high performance liquid chromatography- tandem mass spectrometry (UPLC-MS/MS) to analyze 22 kinds of pesticide residues of zoxamide, pymetrozin, flufenoxuro and so on. Methods The samples were homogenized at high speed and extracted with acetonitrile, and separated by ReproSil 100 C18 (150 mm×2.1 mm, 5 μm) chromatographic column, with the flow rate of 0.3 mL/min and column temperature of 35 ℃, and were quantified by ultra-high performance liquid chromatography-tandem mass spectrometry in a positive ion multiple reaction mode. Results The result showed that excellent linear relationships for 22 pesticides were observed in the concentration range of 0.01-0.2 mg/L with the regression coefficients of 0.9709-0.9998. Under the 3 spiked levels of 0.010, 0.050 and 0.10 mg/kg, the average recovery rates of 22 pesticides were in the range of 71.4%-106.7%, with relative standard deviations of 0.7%-9.9%. The limits of detection and limits of quantitation were 0.90-4.6 μg/kg and 3.0-15.4 μg/kg, respectively. Totally 5 pesticide residues were detected in pear samples. Conclusion The method is simple, rapid and accurate, which can be used for the determination of 22 pesticide residues in pear samples.