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目的建立贝类中扑草净残留量的气相色谱检测方法。方法样品由乙酸乙酯提取,经石墨化碳黑和中性氧化铝双柱串联固相萃取净化,利用DB-1701毛细管色谱柱(30 m×0.53 mm×0.5μm),气相色谱-火焰光度检测器测定。结果该方法在0.10~0.96μg/ml浓度范围内,线性关系良好,相关系数为0.999,检出限为0.0037 mg/kg,定量限为0.010 mg/kg。样品加标回收率为83.7%~102.0%,相对标准偏差为0.54%~8.14%。结论该方法简便、快速、可靠,可用于贝类中扑草净的测定。
Objective To establish a method for the determination of prometryne residues in shellfish by gas chromatography. Methods The sample was extracted with ethyl acetate and purified by two-column solid-phase extraction of graphitized carbon black and neutral alumina. The residue was purified by DB-1701 capillary column (30 m × 0.53 mm × 0.5 μm) Measurement. Results The method showed a good linearity in the concentration range of 0.10-0.96 μg / ml with a correlation coefficient of 0.999. The limit of detection was 0.0037 mg / kg and the limit of quantification was 0.010 mg / kg. The recoveries of spiked samples ranged from 83.7% to 102.0% with relative standard deviations of 0.54% ~ 8.14%. Conclusion The method is simple, rapid and reliable and can be used for the determination of prometryn in shellfish.