QuEChERS-超高效液相色谱-串联质谱法同时测定柚花中317种农药残留量

Simultaneous determination of 317 kinds of pesticide residues in pomelo flowers by ultra performance liquid chromatography-tandem mass spectrometry coupled with QuEChERS

中文关键词:  QuEChERS  超高效液相色谱-串联质谱法  柚花  农药残留

英文关键词:QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry  pomelo flowers  pesticide residues

中文摘要:

      目的 建立QuEChERS前处理法结合超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定柚花中317种农药残留量的方法。方法 柚花样品采用乙腈作为提取剂, 经萃取盐盐析处理, 采用乙二胺-N-丙基硅烷化硅胶(ethylenediamine-N-propylsilane silica gel, PSA)和石墨化炭黑(graphitized carbon black, GCB)作为净化剂, 选用ACQUITY UPLC HSS T3色谱柱, 采用梯度洗脱方式在30 min完成317种目标物质的分析。电喷雾源正离子和负离子同时扫描, 采用多重反应监测(multiple reaction monitoring, MRM)模式、基质匹配标准曲线外标法定量。结果 317种农药在该条件下在2.0~200.0 μg/L质量浓度范围内均线性良好, 相关系数r>0.995, 方法定量限为0.002~0.010 mg/kg, 在低、中、高3个添加水平下的平均回收率为74.3%~120.3%, 相对标准偏差在0.36%~10.00%。结论 该方法具有简单、快速、准确、灵敏等特点, 为柚花中多种农药残留的测定和柚花研制的食品安全地方标准提供了可靠的技术支持。

英文摘要:

      Objective To establish a method for simultaneous determination of 317 kinds of pesticide residues in pomelo flowers by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) coupled with QuEChERS extraction. Methods Pomelo flowers samples were extracted with acetonitrile and salted with extraction salt pack, cleaned up by ethylenediamine-N-propylsilane silica gel (PSA) and graphitized carbon blank (GCB), the analytes were separated on an ACQUITY UPLC HSS T3 column to achieve the separation within 30 min. The 317 kinds of pesticides were detected in electron spray ionization with positive ion mode and electron spray ionization with negative ion mode with multiple reaction monitoring (MRM) mode and quantified by matrix matching curve external standard method. Results The 317 kinds of pesticides in pomelo flowers showed good linearity with correlation coefficients (r) greater than 0.995 within the range of 2.0–200.0 μg/L, and the limits of quantification were 0.002–0.010 mg/kg, the average recoveries at 3 spiked levels were 74.3%–120.3%, and the relative standard deviations were 0.36%–10.00%. Conclusion The method is simple, rapid, accurate and sensitive, can meet the rapid detection requirements of 317 kinds of pesticides in pomelo flowers and provide reliable data support for further standardizing for edible safety evaluation of pomelo flowers.