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[目的]建立固相萃取(SPE)与高效液相色谱法(HPLC)联用检测西瓜中氟唑菌酰羟胺残留的分析方法。[方法]样品经乙腈提取、固相萃取净化后,采用高效液相色谱进行分析。对影响回收率和净化效果的固相萃取操作条件进行研究。[结果]在0.01~5 mg/L质量浓度范围内具有良好的线性关系,相关系数r为0.9999。加标质量分数为0.02、0.2、2 mg/kg时,氟唑菌酰羟胺的平均回收率为79%~84%,相对标准偏差(n=5)为2.4%~3.5%。方法的定量限为0.02 mg/kg。[结论]该方法准确度和灵敏度高、重现性好,适用于西瓜中氟唑菌酰羟胺的残留检测。
[Objective] To establish a method for the determination of halozolomide residues in watermelon by solid phase extraction (SPE) and high performance liquid chromatography (HPLC). [Method] The samples were extracted with acetonitrile and purified by solid phase extraction. The samples were analyzed by high performance liquid chromatography. Solid-phase extraction operating conditions affecting recovery and purification were studied. [Result] There was a good linear relationship in the concentration range of 0.01 ~ 5 mg / L, the correlation coefficient r was 0.9999. The spikedraconazole had an average recovery of 79% -84% and a relative standard deviation (n = 5) of 2.4% -3.5% at spiking levels of 0.02, 0.2 and 2 mg / kg. The limit of quantification for this method is 0.02 mg / kg. [Conclusion] The method has high accuracy and sensitivity, good reproducibility and is suitable for the determination of halozolomide residues in watermelon.