Sancho Juan V, Pozo Oscar J, Zamora Tatiana, Grimalt Susana, Hernández Félix
Analytical Chemistry, Experimental Sciences Department, University Jaume I, E-12071, Castellón, Spain.
J Agric Food Chem. 2003 Jul 16;51(15):4202-6. doi: 10.1021/jf034107s.
A rapid and sensitive liquid chromatography/electrospray ionization/tandem mass spectrometry (LC-ESI-MS-MS) method has been developed for the determination of the plant growth regulator paclobutrazol in pear samples. Extraction was performed with methanol by using a high-speed blender Ultra-Turrax, and 10 microL of pear extract was directly injected in the LC-ESI-MS-MS system without any previous sample treatment. The highest sensitivity of the method was achieved under MS-MS conditions obtaining a limit of detection of 0.7 microg/kg and a quantification limit of 5 microg/kg, with a run time of only 5.5 min. Recoveries for paclobutrazol from spiked pear samples at 0.005, 0.05, and 0.5 mg/kg were around 82-102% with relative standard deviations between 2 and 7%. The method was applied to real treated and untreated samples of pears, using quality control samples as a evaluation of the method reliability. Two MS-MS transitions were selected, one for quantification (294 > 70) and the other for confirmation of the analyte (296 > 70). All the experiments were performed in compliance with good laboratory practices.
已开发出一种快速灵敏的液相色谱/电喷雾电离/串联质谱(LC-ESI-MS-MS)方法,用于测定梨样品中的植物生长调节剂多效唑。使用高速搅拌器Ultra-Turrax以甲醇进行萃取,10微升梨提取物无需任何样品前处理即可直接注入LC-ESI-MS-MS系统。该方法在MS-MS条件下实现了最高灵敏度,检测限为0.7微克/千克,定量限为5微克/千克,运行时间仅为5.5分钟。在0.005、0.05和0.5毫克/千克加标梨样品中,多效唑的回收率约为82-102%,相对标准偏差在2%至7%之间。该方法应用于实际处理和未处理的梨样品,并使用质量控制样品评估方法的可靠性。选择了两个MS-MS跃迁,一个用于定量(294>70),另一个用于确认分析物(296>70)。所有实验均按照良好实验室规范进行。