QuEChERS结合超高效液相色谱-串联质谱法测定苹果中多抗霉素B残留与储藏稳定性

Determination of Polyoxin B Residues in Apple Using QuEChERS-Liquid Chromatography Tandem Mass Spectrometry and Storage Stability

[目的]建立苹果中多抗霉素B残留的QuEChERS-超高效液相色谱串联质谱(UPLC/MS/MS)方法,并进行多抗霉素B在苹果中的储藏稳定性研究。[方法]样品经0.1%甲酸水溶液涡旋提取,经C18(50 mg)净化剂净化后,取上清液离心,过0.22μm滤膜,采用HSS T3色谱柱分离,在正离子模式下UPLC/MS/MS测定。[结果]在0.01~0.5 mg/L质量浓度范围内,多抗霉素B的进样质量浓度与其对应的峰面积间呈良好的线性关系,相关系数r=0.9999,该方法检出限(LOD)为0.01 mg/kg,最低检出质量分数(LOQ)为0.05 mg/kg。在0.05、0.1、0.5 mg/kg质量分数的添加水平下,多抗霉素B在苹果中的平均回收率为70.7%~99.4%,相对标准偏差(RSD)为7.56%~9.05%。[结论]在-20℃储藏条件下,苹果样品中多抗霉素B的平均降解率均小于30%,说明多抗霉素B在苹果样品中至少可以稳定储藏12个月,该方法准确、快速、灵敏度高,可用于苹果中多抗霉素B的残留检测与监测分析。

[Aims]This study aims to develop an analysis method by using QuEChERS-ultra performance liquid chromatography tandem mass spectrometry for determination of polyoxin B in apple.And the storage stability of polyoxin B in apple was conducted as well.[Methods]The samples were extracted by 0.1%formic acid aqueous solution,purified with C18(50 mg),centrifuged to precipitate,and then filtered through a 0.22μm millipore membrane.The sample extract was separated with a HSS T3 column and electrospray ionization mode in positive,detected by UPLC/MS/MS.[Results]When the concentration was in the range of 0.01-0.5 mg/L,the linear correlation coefficients was 0.9999,the limit of detection(LOD)was 0.01mg/kg,the limits of quantitation(LOQ)in those sampleswere 0.05mg/kg.The average recoveries of polyoxin B in apple samples at three spiked levels of 0.05,0.1 and 0.5 mg/kg all ranged from 70.7-99.4%,with the relative standard deviation(RSD)of 7.56-9.05%.[Conclusions]The average degradation rate of polyoxin B in apple was less than 30%at-20℃.It was suggested polyoxin B was stable for 12 months storage under freezing condition.The method is accurate,rapid and sensitive and can be used for residue detection and monitoring analysis of polyoxin B in apple.