QuEChERS-高效液相色谱-串联质谱法检测荔枝中氯虫苯甲酰胺、溴氰虫酰胺及代谢物残留

采用高效液相色谱-串联质谱(HPLC-MS/MS)技术,结合改良的QuEChERS法,建立了同时测定荔枝中氯虫苯甲酰胺、溴氰虫酰胺及代谢物J9Z38残留的分析方法.样品用乙腈提取,以N-丙基乙二胺(PSA)和十八烷基键合硅胶(C18)组合吸附剂净化,采用C18反相色谱柱分离,以V(甲酸水溶液):V(乙腈)=15:85为...

Determination of chlorantraniliprole,cyantraniliprole and its metabolites residues in litchi using QuEChERS and high performance liquid chromatography-tandem mass spectrometry

An analytical method was established for simultaneous determination of chlorantraniliprole, cyantraniliprole and its metabolite J9Z38 in litchi by high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) combined with a modified QuEChERS procedure. The target compounds were extracted from the samples with acetonitrile and then cleaned up with primary secondary amine (PSA) and octadecylsilane (C₁₈). The analytes were separated on a C₁₈ column using V (formic acid aqueous solution) : V (acetonitrile)=15 : 85 as mobile phase and analyzed in multiple reaction monitoring (MRM) mode with positive electrospray ionization (ESI+). Quantitative analysis was performed by external standard method using matrix-matched calibration curves. The results showed that the linearity of the target compounds was good (r >0.99) in the range of 0.005-1 mg/L. The limits of quantification (LOQs) were 0.0005-0.01 mg/kg. The average recoveries of the three pesticides in litchi (whole fruit and pulp) ranged from 76% to 98% at the spiked levels of 0.0005-0.5 mg/kg, with the relative standard deviations of 2.5% to 9.6%. The method was applied for the detection of twenty commercial litchi samples in Guangzhou City. The results showed that the residues of chlorantraniliprole were 0.001-0.01 mg/kg, and neither cyantraniliprole nor its metabolite J9Z38 were found. The proposed method is convenient, effective and rapid, and is suitable for the simultaneous determination of chlorantraniliprole, cyantraniliprole and its metabolite in litchi.