摘要
目的 建立超高效液相色谱-四极杆-飞行时间质谱法(ultra performance liquid chromatography-quadrupole-time-of-flight mass spectrometry,UPLC-Q-TOF/MS)快速筛查蔬菜中乙烯利、草甘膦、草铵膦及其代谢物残留的方法。方法 称取2.0 g蔬菜样品,加入10 mL水,混匀后超声提取20 min,8000 r/min离心5 min,上清液经HLB固相萃取(solid-phase extraction,SPE)柱通过式净化,采用UPLC-Q-TOF/MS检测。以5μmol/L亚甲基二磷酸-0.1%甲酸水溶液和乙腈作流动相进行梯度洗脱,目标物在Poroshell 120 HILIC-Z(100 mm×2.1 mm,2.7μm)色谱柱上分离,电喷雾离子源负离子模式下采用飞行时间质谱一级全扫描-信息依赖采集-子离子扫描(TOF MS-IDA-Product Ion)模式采集。结果 目标化合物在色谱柱上保留较好,建立了包含一级精确质量数、二级碎片质谱及保留时间的高分辨质谱筛查数据库,实现了蔬菜中3种极性农药残留及其代谢物的快速筛查,方法筛查限为0.05 mg/kg。结论 该方法前处理简便快速,准确性好,灵敏度高,可实现蔬菜中乙烯利、草甘膦、草铵膦及其代谢物的定性筛查。
Objective To establish a method for the rapid screening of ethephon,glyphosate,glufosinate-ammonium and their metabolite residues in vegetables by ultra performance liquid chromatography-quadrupole-time-of-flight mass spectrometry(UPLC-Q-TOF/MS).Methods A 2.0 g vegetable sample was weighed,mixed with 10 mL of water,and extracted ultrasonically for 20 minutes.After centrifugation at 8000 r/min for 5 minutes,the supernatant was purified by HLB solid-phase extraction(SPE)column with a pass-through mode and detected with UPLC-Q-TOF/MS.The compounds was separated on a Poroshell 120 HILIC-Z column(100 mm×2.1 mm,2.7µm)using gradient elution with 5μmol/L methylene diphosphate-0.1%formic acid aqueous solution and acetonitrile as mobile phase,and detected using the TOF MS-IDA-Product Ion mode with a negative electrospray ionization source.Results The target compounds showed good retention on the chromatographic column.A high-resolution mass spectrometry screening database containing primary accurate mass,secondary fragment mass spectra,and retention time was established,enabling rapid screening of residues of 3 kinds of polar pesticides and their metabolites in vegetables.The screening limit of the method was 0.05 mg/kg.Conclusion This method features a simple and rapid sample preparation process,along with good accuracy and high sensitivity,and can be used for the rapid screening of ethephon,glyphosate,glufosinate-ammonium and their metabolites in vegetables.
作者
张小刚
王敏
王霞
ZHANG Xiao-Gang;WANG Min;WANG Xia(SCIEX(China),Shanghai 200335,China;Shanghai Center of Agri-products Quality and Safety,Shanghai 201708,China)
出处
《食品安全质量检测学报》
2025年第17期54-60,共7页
Journal of Food Safety and Quality
基金
上海市农业科技创新项目(沪农科T2023324)。
关键词
超高效液相色谱-四极杆-飞行时间质谱法
固相萃取
极性农药
蔬菜
筛查
ultra performance liquid chromatography-quadrupole-time-of-flight mass spectrometry
solid-phase extraction
polar pesticide
vegetable
screening
