QuEChERS-超高效液相色谱-串联质谱法测定柑橘中呋虫胺和螺虫乙酯残留量

Determination of dinotefuran and spirotetramat residue in citrus by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  呋虫胺  螺虫乙酯  柑橘  残留

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  dinotefuran  spirotetramat  citrus  residues

中文摘要:

      目的 建立QuEChERS-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC－MS/MS) 同时测定柑橘中呋虫胺及螺虫乙酯残留量的分析方法。方法 样品采用QuEChERS方法, 经1%甲酸乙腈涡旋振荡提取, 无水硫酸镁和氯化钠盐析后, 经乙二胺-N-丙基硅烷、C18混合净化剂净化, 用Waters ACQUITY UPLC HSS T3色谱柱分离, 超高效液相色谱-串联质谱正离子扫描、多反应监测模式进行测定, 外标法定量。结果 呋虫胺及其代谢物、螺虫乙酯及其代谢物在相关浓度范围内线性关系良好, 相关系数均大于0.99。呋虫胺及其代谢物的回收率为86.8%~97.6%, 相对标准偏差为2.7%~6.8%, 方法定量限为0.005~0.01 mg/kg; 螺虫乙酯及其代谢物的回收率为85.8%~96.9%, 相对标准偏差为3.2%~7.4%, 方法定量限为0.005~0.008 mg/kg。结论 该方法样品前处理过程简单快速, 分析时间短, 定量限低、正确度及精密度均符合农药残留检测要求, 适用于同时测定柑橘中呋虫胺和螺虫乙酯残留。

英文摘要:

      Objective To establish a method for simultaneous determination of dinotefuran and spironolactone residues in citrus by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted by QuEChERS method, extracted by 1% acetonitrile carboxylic acid, salted out by anhydrous magnesium sulfate and sodium chloride, purified by ethylenediamine-n- propyl silane and C18 mixed purifier, separated by Waters ACQUITY UPLC HSS T3 chromatographic column, determined by UPLC-MS/MS positive ion scanning and multi-reaction monitoring mode, and quantified by external standard method. Results The furanid and its metabolites, spirotetramat and its metabolites had a good linear relationship in the relevant concentration range, and the correlation coefficients were greater than 0.99. The recoveries of furfuran and its metabolites were 86.8%97.6%, the relative standard deviations were 2.7%6.8%, and the limits of quantification were 0.0050.01 mg/kg. The recoveries of spirotetramat and its metabolites were 85.8%96.9%, the relative standard deviations were 3.2%7.4%, and the limits of quantification were 0.0050.008 mg/kg. Conclusion This method has simple and fast sample preparation process, short analysis time, low limit of quantification, accuracy and precision, which meet the requirements of pesticide residue detection, and is suitable for simultaneous determination of furfuran and spirotetrame residues in citrus.