HPLC-MS/MS法测定植物油中氟吡甲禾灵和高效氟吡甲禾灵

建立了一种利用固相萃取-液相色谱质谱联用法测定植物油中氟吡甲禾灵和高效氟吡甲禾灵的方法。试样用乙腈提取,提取液经PSA/Silic复合填料固相萃取柱净化,使用液相色谱质谱联用仪检测,监测的特征离子对为376/316和376/288,根据色谱峰的保留时间及特征离子对定性,外标法定量。此方法在0.010~0.500 μg/mL的相关系数为0.9999,在0.010、0.10 μg/mL和0.50 μg/mL添加水平的回收率为86.3%~108.2%,响应值相对标准偏差为2.05%~2.72%(n=6),方法检出限为0.0012 mg/kg。该方法简单、准确、灵敏度高,适合于植物油中氟吡甲禾灵和高效氟吡甲禾灵的检测。

Determination of Haloxyfop-Methyl and Haloxyfop-P in Vegetable Oil by High Performance Liquid Chromatography-Tandem Mass Spectrometry

A method for the determination of haloxyfop-methyl and haloxyfop-P in vegetable oil by solid phase extraction liquid chromatography mass spectrometry was established.The sample was extracted with acetonitrile,and the extract was purified by PSA/silic composite packing solid phase extraction column.The characteristic ion pairs were 376/316 and 376/288,which were determined by retention time of chromatographic peaks and characteristic ion pairs detected by multiple reactions,and quantified by external standard method.The linear range of the method was 0.010~0.500 μg/mL and the correlation coefficient was 0.9999.The recoveries were 86.3%~108.2% at the addition levels of 0.010,0.10 and 0.50 μg/mL,the relative standard deviations of the response values ranged from 2.05%~2.72% (n=6),and the detection limit was 0.0012 mg/kg.The method is simple,accurate and sensitive,and is suitable for the determination of haloxyfop-methyl and haloxyfop-P in vegetable oil.