反相高效液相色谱法检测大豆中咪草烟.PDF

※分析检测 食品科学 2010, Vol. 31, No. 08 237 周艳明，张寒松，赵瑛博，朱 君 (沈阳农业大学分析测试中心，辽宁沈阳 110161) ：建立大豆中咪草烟残留量测定的高效液相色谱方法，并对所建立的方法进行可靠性分析。甲醇-0.1mol/L 碳酸钠溶液(50:50 ，V/V)超声提取，离心，上清液调酸后用二氯甲烷萃取，强阳离子交换固相萃取柱净化，收集 的洗脱液蒸干后用1mL 甲醇溶解，配有紫外检测器的高效液相色谱仪测定，对该方法的灵敏度、准确度和精密度 进行验证实验。咪草烟的检出限为0.00837mg/kg 。各浓度水平的平均添加回收率范围为70.6%～106.7%、相对标 准偏差范围为1.56%～12.8%。所建立的大豆中咪草烟残留量测定方法符合国家标准对食品中农药残留测定的要求。 ：咪草烟；高效液相色谱( H P L C ) ；残留；大豆 Reversed-phase HPLC Determination of Imazethapyr in Soybeans ZHOU Yan-ming ，ZHANG Han-song ，ZHAO Ying-bo ，ZHU Jun (Analysis and Testing Center, Shenyang Agricultural University, Shenyang 110161, China) Abstract ：A reversed-phase high-performance liquid chromatographic (RP-HPLC) method was proposed for the determination of imazethapyr in soybeans and its reliability was evaluated by determining various figures of merit such as sensitivity, accuracy and precision. Samples were extracted using a mixture of methanol and 0.1 mol/L sodium carbonate aqueous solution with ultrasonic assistance and centrifugated. The supernatant was then harvested, acidified and extracted twice using methylene chloride. The methylene chloride phase was finally separated using a separatory funnel and cleaned up on a strong cation exchange solid-phase extraction column and the resulting eluate was evaporated to dryness and redissolved in methanol prior to injection into the HPLC system equipped with a UV detector. The method revealed a limit of detection of 0.00837 mg/kg. Mean recoveries of 3 replicates for imazethapyr in 4 varieties of soybeans spiked at 3 levels were within the range of 70.6% －106.7%, with a RSD range of 1.56% －12.8%. This method proved to meet the Chinese national standard requirements for the determination of pesti