液相色谱–质谱联用测定咖啡中肟菌酯及代谢物残留

张蕊; 邓露晴; 李祥英; 赵俊龙; 李梓琳; 凡帅; 刘承兰

doi:10.7671/j.issn.1001-411X.201804002

液相色谱–质谱联用测定咖啡中肟菌酯及代谢物残留

Determination of trifloxystrobin and its metabolite in coffee by liquid chromatography-mass spectrometry

摘要

摘要:
目的建立一种同时测定咖啡中肟菌酯及其代谢物肟菌酸残留量的液相色谱–质谱检测方法。

方法样品中待测农药组分采用含φ为1%乙酸的乙腈匀浆后超声提取，氯化钠和无水硫酸镁盐析及高速离心后，取上清液经C₁₈分散固相萃取净化，采用液相色谱–质谱联用检测，ESI (+)电离和多反应监测(MRM)定量测定。

结果添加肟菌酯质量分数为0.01~2.00 mg·kg^–1时，肟菌酯在咖啡全果中的添加回收率为87.8%~106.7%，相对标准偏差(RSD)为1.3%~5.8%；在咖啡豆中添加回收率为83.2%~88.1%，RSD为2.0%~6.2%。肟菌酸在咖啡全果中的添加回收率为71.5%~106.0%，RSD为1.0%~6.1%；在咖啡豆中的添加回收率为84.4%~105.2%，RSD为1.0%~5.2%。肟菌酯及肟菌酸在咖啡中的最小检出量均为2.5×10^–12 g，最低检出限均为0.01 mg·kg^–1。

结论该方法操作简便、快速和稳定，可以满足咖啡实际样品中肟菌酯及其代谢物肟菌酸的残留检测要求。

Abstract:
Objective To develop a method for determining trifloxystrobin and its metabolite trifloxystrobin acid simultaneously in coffee by liquid chromatography-mass spectrometry (LC-MS).

Method The sample was ultrasonically extracted with acetonitrile (including φ=1% acetic acid), and salted out with sodium chloride and anhydrous magnesium sulfate. After high-speed centrifugation, the supernatant was purified by C₁₈ dispersive solid-phase extraction and detected by LC-MS. The quantitative determination was conducted by ESI (+) ionization mode and multi-reaction monitoring (MRM).

Result The recovery rates of trifloxystrobin in coffee fruits ranged from 87.8% to 106.7%, and the relative standard deviation (RSD) ranged from 1.3% to 5.8% when the additive amount of trifloxystrobin ranged from 0.01 to 2.00 mg·kg^–1. The recovery rates of trifloxystrobin in coffee beans ranged from 83.2% to 88.1%, and the RSD ranged from 2.0% to 6.2%. The recovery rates of trifloxystrobn acid in coffee fruits ranged from 71.5% to 106.0%, and the RSD ranged from 1.0% to 6.1%. The recovery rates of trifloxystrobn acid in coffee beans ranged from 84.4% to 105.2%, and the RSD ranged from 1.0% to 5.2%. The minimum detectable amounts of both trifloxystrobin and trifloxystrobin acid in coffee were 2.5 × 10^–12 g, and the minimum limits of quantitation were 0.01 mg·kg^–1.

Conclusion This method is simple, rapid and stable, and can meet the requirement for detecting the residues of trifloxystrobin and its metabolites in coffee samples.

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