Chen Xixi, Xu Jun, Liu Xingang, Tao Yan, Pan Xinglu, Zheng Yongquan, Dong Fengshou
State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing, P.R. China.
J Sep Sci. 2014 Jul;37(13):1640-7. doi: 10.1002/jssc.201400157.
A sensitive analytical method for the simultaneous determination of trifloxystrobin and its metabolite trifloxystrobin acid in rice including straw, bran, brown rice and soil was developed by using ultra high performance liquid chromatography coupled with tandem mass spectrometry. The fungicide trifloxystrobin and its metabolite trifloxystrobin acid were extracted using acetonitrile with 1% formic acid v/v and subsequently cleaned up by primary secondary amine, octadecylsilane or graphitized carbon black prior to ultra high performance liquid chromatography coupled with tandem mass spectrometry. The determination of two target compounds was achieved in less than 3 min using an electrospray ionization source in positive mode. The limits of detection were below 0.22 μg/kg and the limits of quantification did not exceed 0.74 μg/kg in all matrices, which were much lower than the maximum residue levels established by the Codex Alimentarius Commission. The overall average recoveries in four matrix at three levels (0.1, 1.0 and 5.0 mg/kg) ranged from 74.2 to 107.4% with a relative standard deviations of less than 7.8% (n = 5) for both analytes. The method was demonstrated to be convenient and reliable for the routine monitoring of trifloxystrobin and its metabolite. The developed method was validated and applied for the analysis of degradation study samples.
采用超高效液相色谱-串联质谱法,建立了一种同时测定水稻(包括稻草、米糠、糙米)和土壤中肟菌酯及其代谢产物肟菌酸的灵敏分析方法。用含1%(体积比)甲酸的乙腈提取杀菌剂肟菌酯及其代谢产物肟菌酸,然后在进行超高效液相色谱-串联质谱分析之前,通过伯仲胺、十八烷基硅烷或石墨化炭黑进行净化。使用电喷雾电离源正模式,在不到3分钟的时间内实现了两种目标化合物的测定。所有基质中的检测限均低于0.22μg/kg,定量限均不超过0.74μg/kg,远低于食品法典委员会规定的最大残留限量。在三个添加水平(0.1、1.0和5.0mg/kg)下,四种基质中的总平均回收率在74.2%至107.4%之间,两种分析物的相对标准偏差均小于7.8%(n = 5)。该方法被证明对于肟菌酯及其代谢产物的常规监测既方便又可靠。所建立的方法经过验证,并应用于降解研究样品的分析。