Ding Ming, Zhong Donglian, Tang Fubin, Fang Wei
Research Institute of Subtropical Forestry, Chinese Academy of Forestry, Fuyang 311400, China.
Se Pu. 2013 Feb;31(2):117-21. doi: 10.3724/sp.j.1123.2012.10005.
A simple and efficient method based on solid-phase extraction (SPE) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed for the determination of butylene fipronil, chlorpyrifos, chlorantraniliprole, fipronil, imidacloprid, indoxacarb and phoxim residues in bamboo shoots. The sample was extracted with acetonitrile and purified by a primary secondary amine (PSA) solid-phase extraction cartridge. The detection of targets was performed by HPLC-MS/MS with multiple reaction monitoring (MRM) mode. All the seven pesticides were completely separated in 15 min with an excellent linear relationship. The limits of detection and the limits of quantification for the seven pesticides were 0.02-0.5 microg/kg and 0.08-1.5 microg/kg, respectively. The recoveries of the seven pesticides spiked in a bamboo shoot sample at the levels of 4, 8, 32 microg/kg were in the range from 76.0% to 102.6% (the RSD < or = 11.0%, n = 3). The method was successfully applied to the real bamboo shoot samples. The method has high accuracy and sensitivity, and is simple and quick. It can meet the requirement of the simultaneous determination of the seven pesticides in bamboo shoots.
建立了一种基于固相萃取(SPE)和高效液相色谱-串联质谱(HPLC-MS/MS)的简单高效方法,用于测定竹笋中丁烯氟虫腈、毒死蜱、氯虫苯甲酰胺、氟虫腈、吡虫啉、茚虫威和辛硫磷的残留量。样品用乙腈提取,并用伯仲胺(PSA)固相萃取柱净化。采用HPLC-MS/MS的多反应监测(MRM)模式对目标物进行检测。7种农药在15分钟内完全分离,线性关系良好。7种农药的检出限和定量限分别为0.02 - 0.5微克/千克和0.08 - 1.5微克/千克。在竹笋样品中添加4、8、32微克/千克水平的7种农药,回收率在76.0%至102.6%之间(相对标准偏差RSD≤11.0%,n = 3)。该方法成功应用于实际竹笋样品的检测。该方法具有高准确性和高灵敏度,且简单快速。它能够满足同时测定竹笋中7种农药的要求。