【摘 要】
：
建立了大米中甲萘威农药残留量的固相萃取-高效液相色谱(SPE-HPLC)分析方法。以乙腈为提取剂,振荡提取,采用C_(18)固相萃取柱净化,经C_(18)柱(3.9 mm×300 mm,10μm)分离,乙
【机 构】
：
宁夏粮油产品质量检测中心,宁夏大学,
论文部分内容阅读
建立了大米中甲萘威农药残留量的固相萃取-高效液相色谱(SPE-HPLC)分析方法。以乙腈为提取剂,振荡提取,采用C_(18)固相萃取柱净化,经C_(18)柱(3.9 mm×300 mm,10μm)分离,乙腈-水(55︰45,V/V)为流动相,柱温40℃,流速1.0 m L/min进行分离,紫外检测器280 nm下进行检测。甲萘威的质量浓度在0.05~2.00μg/mL范围内线性良好,相关系数为0.999 9。在0.50,1.25和2.50 mg/kg 3个添加水平下,甲萘威的加标回收率为92.41%~110.18%,相对标准偏差在2.91%~4.35%(n=6),检出限为0.006 mg/kg。该方法具有样品前处理操作简单、灵敏度高、试剂用量少、重现性好等优点,适用于大米中甲萘威的定性定量分析。
A solid phase extraction and high performance liquid chromatography (SPE-HPLC) method for the determination of carbaryl in rice was established. The acetonitrile - water (55:45, V / V) solution was extracted with acetonitrile and purified by C_ (18) solid phase extraction column and separated on a C 18 column (3.9 mm × 300 mm, 10 μm) The mobile phase was separated at a column temperature of 40 ℃ and a flow rate of 1.0 mL / min, and detected by UV detector at 280 nm. Carbaryl mass concentration in the range of 0.05 ~ 2.00μg / mL good linearity, the correlation coefficient of 0.999 9. The recoveries of carbaryl ranged from 92.41% to 110.18% with relative standard deviations (RSDs) ranging from 2.91% to 4.35% (n = 6) at the three addition levels of 0.50, 1.25 and 2.50 mg / kg with a detection limit of 0.006 mg / kg. The method has the advantages of simple sample pretreatment, high sensitivity, less reagent usage, good reproducibility and the like, and is suitable for the qualitative and quantitative analysis of carbaryl in rice.
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