QuEChERS-UPLC-MS/MS法测定热带和亚热带水果中5种三唑类杀菌剂

该实验采用QuEChERS净化-超高效液相色谱-串联质谱法测定石榴、芒果、火龙果的5种三唑类杀菌剂残留。样品10.0 g经改进的QuEChERS方法进行前处理，采用ZORBAX SB-C18色谱柱分离，以4 mmol/L甲酸水溶液和甲醇为流动相进行梯度洗脱。质谱采用电喷雾离子源（ESI）和多反应监测（MRM）模式。5种三唑类杀菌剂的质量浓度为4.0～200.0 μg/L时，线性关系良好，相关系数（R2）＞0.999，定量限（LOQ）为0.15～1.0 μg/kg，石榴、芒果、火龙果中5种三唑类杀菌剂加标回收率分别为87.7%～103.1%、80.5%～93.5%、81.6%～94.7%，相对标准偏差（RSD）（n=6）分别为4.1%～11.2%、3.8%～7.3%、4.3%～10.2%。说明该方法灵敏度及准确度良好，能满足石榴、芒果、火龙果（皮不可食的热带和亚热带水果）中5种三唑类杀菌剂残留检测的要求。

Determination of 5 kinds of triazole fungicides residues in tropical and subtropical fruits byQuEChERS with UPLC-MS/MS

Five kinds of triazole fungicides residues in pomegranate,mango and pitaya were determined by QuEChERS purification with ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).10.0 g samples were pretreated with improved QuEChERS method,and then the target analytes were separated on ZORBAX SB-C₁₈column with gradient elution using mobile phase made up of 4 mmol/L formic acid aqueous solution and methanol.Electrospray ionization(ESI)and multiple reaction monitoring(MRM)mode were adopted in MS analysis.5 kinds of triazole fungicides showed good linearity in the concentration range of 4.0-200.0μg/L,and the correlation coefficient(R2)was greater than 0.999.The limits of detection(LOQ)were 0.15-1.0μg/kg,the standard recovery rates of 5 kinds of triazole fungicides residues in pomegranate,mango and pitaya were 87.7%-103.1%,80.5%-93.5%,and 81.6%-94.7%,respectively.The relative standard deviations(RSDs)(n=6)were 4.1%-11.2%,3.8%-7.3%,and 4.3%-10.2%,respectively.The method was sensitive and accurate,which could meet the requirements for the determination of 5 kinds of triazole fungicides residues in pomegranate,mango and pitaya(tropical and subtropical fruits with inedible peel).