QuEChERS EMR-Lipid净化结合同位素稀释-超高效液相色谱-串联质谱法同时测定蜂房及其制剂中10种真菌毒素

Simultaneous Determination of Ten Mycotoxins in Vespae Nidus and Its Preparations by QuEChERS EMR-Lipid Combined with Isotope Dilution-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

目的 建立一种Qu ECh ERS EMR-Lipid净化结合同位素稀释-超高效液相色谱-串联质谱技术(UPLC-MS/MS)同时测定蜂房及其制剂中10种真菌毒素的检测方法。方法 样品经80%乙腈水溶液提取,Qu ECh ERS EMRLipid净化,采用UPLC-MS/MS,在多反应监测(MRM)模式下进行测定,内标法定量。结果 10种真菌毒素含量在各自质量浓度范围内具有较好的线性关系(r>0.999),目标化合物在低、中、高3个质量浓度下的平均回收率为83.8%~107.1%(RSD<6.5%),定量限(LOQ)为0.18~129μg/kg。结论 该法前处理步骤简便,净化效果良好,提高了样品检测效率,内标法定量精准可靠,适用于蜂房及其制剂中10种真菌毒素的同时检测。

Objective To establish a method for simultaneous determination of ten mycotoxins in Vespae Nidus and its preparations by QuEChERS EMR-Lipid combined with isotope dilution-ultra performance liquid chromatographytandem mass spectrometry(UPLC-MS/MS).Methods The samples were extracted with 80 % acetonitrile solution and purified by QuEChERS EMR-Lipid.Ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was used for determination in mode of multiple reaction monitoring(MRM),and internal standard method was used for quantification.Results The 10 mycotoxins showed good linearity within their respective concentration range(r>0.999).The average recoveries were 83.8 %-107.1 %(RSDs<6.5 %) at low,medium,and high spiked levels.The LOQs were in the range of 0.18-129 μg/kg.Conclusion The method has simple pretreatment steps,good purification effect,and improved sample detection efficiency,and the internal standard method is accurate and reliable.It is suitable for simultaneous detection of 10 mycotoxins in Vespae Nidus and their preparations.