气相色谱法测定蔬菜、水果中特丁硫磷砜和特丁硫磷亚砜残留量

摘要

建立蔬菜、水果中特丁硫磷砜和特丁硫磷亚砜残留量的测定方法。样品经匀浆后，经含氯化钠的乙腈震荡提取，取乙腈层浓缩至近干，用丙酮进行溶解定容，采用DB－1701毛细管色谱柱（30 m ×0．25 mm ×0．25μm）分离，经气相色谱仪检测。在优化的气相色谱条件下，特丁硫磷砜和特丁硫磷亚砜分离良好，其含量分别在0．137～1．37μg／mL、1．39～13．9μg／mL浓度范围内线性关系良好，相关系数均大于0．998，加标回收率为82．1％～107．6％，相对标准偏差（RSD，n＝6）为3．4％～6．8％。该方法灵敏、准确、可靠，能准确的测定蔬菜和水果中的特丁硫磷砜和特丁硫磷亚砜，具有分析时间短、抗干扰性好、定量准确等优点，可为全面实现对蔬菜和水果中的特丁硫磷总量进行监测提供检测依据。%To establish a capillary gas chromatography method for the determination of Terbufos -sulfone and Terbufos -sulfoxide in vegetables and fruit .The sample were homogenized , then extracted by acetonitrile with sodium chloride , and evaporated to near dryness , dissolved and constant volume with acetone .The sample was separate by DB -1701 column (30 m ×0.32 mm ×0.25 μm), then detected by gas chromatography .Terbufos-sulfone and Terbufos -sulfoxide have good resolution and linear relationship within 0.137 ~1.37μg/mL、1.39 ~13.9μg/mL concentration range under the optimum conditions.The spiked recoveries were in the range of 82.1%~107.6%with relative standard deviations (RSDs, n=6) of 3.4%~6.8%.The method has the advantages of short peak retention , high sensitivity, accurate, reliable, good reproducibility and selectivity , which can accurate determinated of Terbufos sulfone and Terbufos sulfoxide in fruits and vegetables and can detection basis for comprehensive monitoring the content of the total Terbufos in fruits and vegetables .