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
胡珀 1卜媛媛 1金鹏 1何晓希 2赵祥杰2
作者信息
- 1. 淮安市食品药品检验所,江苏 淮安 223001
- 2. 淮阴工学院,江苏 淮安 223001
- 折叠
摘要
目的 建立一种QuEChERS 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,QuEChERS EMR-Lipid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0.18～129 μg/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.
Abstract
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 chromatography-tandem 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.
关键词
QuEChERS/EMR-Lipid/蜂房/真菌毒素/超高效液相色谱-串联质谱法/同位素内标Key words
QuEChERS EMR-Lipid/Vespae Nidus/mycotoxin/ultra performance liquid chromatograph-tandem mass spectrometry(UPLC-MS/MS)/isotope internal standard引用本文复制引用
基金项目
江苏省市场监督管理局科技计划项目(KJ2022048)
出版年
2024
NETL
NSTL
万方数据