柑橘及土壤中高效氯氟氰菊酯残留分析方法研究

【目的】建立快速、实用的测定柑橘及土壤中高效氯氟氰菊酯残留的方法。【方法】样品经甲醇提取、弗罗里硅土柱净化、浓缩、定容后，用带μ-ECD检测器的气相色谱仪进行测定。【结果】高效氯氟氰菊酯在0.005~1.000 μg/mL范围内线性良好，线性相关系数r＝0.9996。该方法对高效氯氟氰菊酯标样的最小检出限为1.0×10-12 g，对橘皮、橘肉和土壤的最低检出浓度均为0.001 mg/kg，样品平均回收率为90.96%~104.21%，相对标准偏差为2.73%~10.45%。【结论】建立的GC-μECD检测方法具有分离效果好、回收率高、经济快速、准确度和灵敏度高的特点，适用于柑橘及土壤中高效氯氟氰菊酯的残留检测。

Analytical method for detecting 1ambda-cyhalothrin residues in citrus fruits and soil

[Objective]The goal of this experiment was to develop a rapid method for detecting lambda-cyhalothrin residues in citrus fruits and soil. [Method]The samples were extracted with methanol, cleaned up and concentrated on a florisil column, and analyzed by GC using μ-ECD. [Result]The linear relationship of lambda-cyhalothrin was found better in the concentration range from 0.005 to 1.000 μg/mL with the linear correlation coefficient of 0.9996. Minimum limit of detection in standard samples was recorded as 1.0×10-12 g in the present method, the lowest detectable concentration in citrus peel, pulp, and soil samples was 0.001 mg/kg. The average recovery varied from 91.24 to 104.61%, and the relative standard deviation ranged from 2.73 to 10.45%. [Conclusion]Owing to its good isolation effect, high recovery rate, rapidness, accuracy and high sensitivity, the GC method using μECD is immensely applicable to detect the lambda-cyhalothrin residues in citrus fruits and soil.