不同前处理方法对霉千张中赭曲霉毒素A检测效果对比
目的 考察不同的固相萃取柱的净化效果, 建立超高效液相色谱——串联质谱法检测霉千张中赭曲霉毒素A的检测方法。方法 样品经甲醇+水(80:20, V:V)提取, 萃取柱净化, 目标化合物在多反应监测模式下进行检测, 以基质匹配标准曲线法进行定量。优化色谱与质谱条件后, 从回收率、基质效应、净化效率3个方面考察了HLB、C18、MAX和免疫亲和柱, 对霉千张中赭曲霉毒素A残留净化效果的影响。结果 HLB、C18、免疫亲和柱、MAX固相萃取柱的基质效应分别为0.83、0.78、0.84、0.67; 净化效率为75.6%、70.8%、81.5%、50.2%。赭曲霉毒素A在0.10～10.0 ng/mL范围内线性关系良好, 相关系数为0.9998, 加标回收率为86.0%～104.8%, 相对标准偏差为1.2%～6.8%, 方法的检出限为0.10 μg/kg。结论 HLB, C18和免疫亲和柱均有较好的净化效果, 免疫亲和柱和HLB价格昂贵, 不太适合大批量样本的检测, 因此选择C18作为霉千张样品的前处理固相萃取柱。该方法前处理简单, 选择性好, 灵敏度高, 适用于霉千张中赭曲霉毒素A的测定。
Objective To investigate the purification effects of different solid-phase extraction columns and establish a method for the determination of ochratoxin A in fermented dried beancurd sheet by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with methanol + water (80:20, V:V), purified by an extraction column, and the target compounds were detected in multiple reaction monitoring mode, quantified by matrix-matched standard curve method. After optimizing the chromatogram and mass spectrometry, the effects of HLB, C18, MAX and immunoaffinity column on the purification effect of ochratoxin A residues in mildew were investigated from three aspects: recovery, matrix effect and purification efficiency. Results The matrix effects of HLB, C18, immunoaffinity columns, and MAX solid-phase extraction columns were 0.83, 0.78, 0.84 and 0.67, respectively; purification efficiency was 75.6%, 70.8%, 81.5% and 50.2%. Ochratoxin A had a good linear relationship in the range of 0.10-10.0 ng/mL, with the correlation coefficient of 0.9998. The standard recoveries were 86.0%-104.8%, the relative standard deviations were 1.2%-6.8%, and the limit of detection was 0.10 μg/kg. Conclusion HLB, C18 and immunoaffinity columns all have better purification effect. Immunoaffinity columns and HLB are expensive and are not suitable for the detection of large quantities of samples. Therefore, C18 was selected as the pre-treatment solid phase extraction column for fermented dried beancurd sheet. This method is simple, selective and sensitive, and is suitable for the determination of ochratoxin A in fermented dried beancurd sheet.
标题：不同前处理方法对霉千张中赭曲霉毒素A检测效果对比
英文标题：Comparison of detection effect of ochratoxin A in fermented dried beancurd sheet by different sample pretreatments
作者：
高何刚 绍兴市疾病预防控制中心
杜赛 绍兴市疾病预防控制中心
王若燕 绍兴市疾病预防控制中心
陈理 绍兴市疾病预防控制中心
周临 绍兴市疾病预防控制中心
中文关键词:霉千张,赭曲霉毒素A,固相萃取,超高效液相色谱串联质谱法,
英文关键词:fermented dried beancurd sheet,ochratoxin A,solid phase extraction,ultra performance liquid chromatography-tandem mass spectrometry,
发表日期：2019-11-06
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