UPLC-MS/MS测定蜂王浆中7种磺胺类药物的残留

王伟; 尤翠萍

doi:10.3969/j.issn.1673-159X.2019.03.013

UPLC-MS/MS测定蜂王浆中7种磺胺类药物的残留

王伟,
尤翠萍

Determination of Seven Kinds of Sulfonamides Residues in Royal Jelly by UPLC-MS/MS

摘要

摘要:
目的建立超高效液相色谱-串联质谱法测定蜂王浆中磺胺类药物残留的方法。
方法试样加入乙腈-水(V_乙腈:V_水=80:20)溶液提取，经HLB固相萃取柱净化后，用超高效液相色谱-串联质谱分析测定。选用乙腈-0.1%甲酸为流动相，多反应监测模式(MRM)分析目标化合物。
结果7种磺胺类药物均有良好线性关系，相关系数均大于0.99，检出限为0.5~8.0 μg/kg，定量限为1.0~10.0 μg/kg，加标回收率为79.29%~102.63%，相对标准偏差为2.5%~8.4%。
结论该方法灵敏度高、操作方便，适用于蜂王浆中7种磺胺类药物残留同时、快速检测。

Abstract:
ObjectiveTo establish a method of ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) for the simultaneous determination of seven kinds of sulfonamides.
MethodsAfter honey was extracted by acetonitrile:water(80:20), the extraction was quickly purified by HLB and analyzed by UPLC-MS/MS.The qualitative and quantitative analysis of the compounds was carried out under the multi-reaction monitoring(MRM) modein matrix-matched standard method.
ResultsIt shows a good linearity(r²>0.99) for all compounds.The LOD values of antibiotics and pesticides were in the range of 0.5~8.0 μg/kg.The LOQs of antibiotics and pesticides were in the range of 1.0~10.0 μg/kg.At the three spiking levels, the recoveries ranged in 79.29%~102.63% with relative standard deviations of 2.5%~8.4%.
ConclusionThe proposed method was simple, rapid, sensetive and accurate, and it could fit for the requirements of residue analysis.

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