超高效液相色谱串联质谱法测定溴虫氟苯双酰胺及其两种代谢物在辣椒上的残留

Simultaneous determination of broflanilide and its two metabolites in capsicum by ultra-high performance liquid chromatography-tandem mass spectrometry

本研究建立并优化了基于超高效液相色谱串联质谱(UHPLC-MS/MS)同时测定辣椒中溴虫氟苯双酰胺及其代谢物DM-8007和S(PFP-OH)-8007的残留分析方法。样品经过乙腈提取,无水硫酸镁、N-丙基乙二胺(PSA)及石墨化炭黑(GCB)净化。净化样品以甲醇和0.2%甲酸水为流动相,采用C18色谱柱进行分离,并通过电喷雾正离子(ESI+)扫描,多反应监测(MRM)模式进行定量分析。结果表明,溴虫氟苯双酰胺及其两种代谢物在0.01~1 mg/kg范围内与目标化合物的峰面积线性关系良好,相关系数均大于0.99;在空白辣椒基质中添加溴虫氟苯双酰胺及其两种代谢物,在3个加标水平下回收率为90.8%~97.4%,相对标准偏差(RSD)为1.3%~5.7%,定量限(LOQ)为0.01 mg/kg,满足残留分析的要求。采用该方法监测了5%溴虫氟苯双酰胺悬浮剂在湖南、河南、浙江3个地点的消解动态,溴虫氟苯双酰胺在辣椒样品中的消解动态规律符合一级反应动力学方程,在3个地点的半衰期分别为7.7、4.7 d和2.8 d。

An analytical method for simultaneous determination of broflanilide and its two metabolites DM-8007 and S(PFP-OH)-8007 in capsicum samples by ultra-performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)was established.Capsicum samples were extracted with acetonitrile and purified by matrix dispersion extraction with anhydrous magnesium sulphate,N-propyl ethylenediamine(PSA)and graphitized carbon black(GCB)as adsorbents.The purified sample was separated on a C18 chromatographic column using methanol and 0.2%formic acid water as mobile phase.Samples were detected using positive electrospray ionization(ESI+)under MRM mode.The results showed that a good linear relationship between the peak area of target compound and their concentration ranging from 0.01-1 mg/kg was obtained with the correlation coefficients all higher than 0.99.The average recoveries of broflanilide and its two metabolites in capsicum at three spiked levels were 90.8%-97.4%,with a RSD value of 1.3%-5.7%,and the limit of quantitative(LOQ)was 0.01 mg/kg.The degradation dynamics of broflanilide 5%suspension concentrate in Hunan,Henan,and Zhejiang were monitored,showing that the degradation dynamics of broflanilide in capsicum samples conformed to the first-order reaction kinetics equation.The half-life of of broflanilide in capsicum were 7.7,4.7 d and 2.8 d in the three sites,respectively.