74 - 食品科学技术页

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Determination of Four Anticoagulant Rodenticides Residues in
Vegetables and Fruits using QuEChERS鄄UPLC鄄MS / MS
SONG Wei,摇 YANG Baichong,摇 ZHAO Yongbiao,摇 SONG Guixue*
( Pony Testing Co. Ltd. , Beijing 100082, China )
Abstract: Using the QuEChERS pretretment, a method was established to detect warfarin, coumatetra鄄
lyl, brodifacoum, and flocoumafen in vegetables and fruits with ultra high performance liquid chromatog鄄
raphy鄄tandem mass spectrometry ( UPLC鄄MS / MS) . Grounded and homogenized samples were extracted
using acetonnitrile containing 1% ( V / V ) glacial acetic acid in Waters DisQue tubes and cleaned up.
Components in the supernatant were separated by an UPLC BEH C18 column and eluted by methanol and
5 mmol / L ammonium acetate and 0郾 1% ( V / V) formic acid solution with gradient elution. Analysis was
accomplished by ESI鄄[ M鄄H] - with a multiple reaction monitor ( MRM) mode and external standard
quantification. In order to eliminate matrix effect, DisQue purification tubes with additional PSA and
GCB, were tested and discussed. The results showed that 5 mg GCB had good effects. Moreover, warfa鄄
rin and coumatetralyl were in a linear corelation with the range of 0郾 5 - 100 滋g / L and the detection of
limits (LOD) was 0郾 25 滋g / kg. Brodifacoum and flocoumafen were in a linear correaltion with the range
of 2 - 250 滋g / L and the LOD was 1郾 0 滋g / kg. Spiked recoveries at low, medium, and high concentration
levels were in the range of 86% - 128% with RSD of 2郾 4% - 16% .
Key words: anticoagulant rodenticides; residues in vegetables and fruits; marfarin; coumatetralyl; brod鄄
ifacoum; flocoumafen
( 责任编辑: 李摇 宁)
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第 32 卷 第 3 期摇 摇 摇 摇 摇 摇 摇 宋摇 薇等: QuEChERS鄄UPLC鄄MS / MS 测定果蔬中 4 种残留抗凝血杀鼠剂