免疫亲和柱净化-液相色谱-串联质谱法同时测定水产品中8种霉菌毒素

目的:建立免疫亲和柱净化-液相色谱-串联质谱法(LC-MS/MS)同时测定水产品中8种霉菌毒素残留。方法:样品经乙腈水溶液(84:16,V:V)提取,多毒素免疫亲和柱净化。色谱柱为Agilent Proshell 120 SB·C₁₈(2.1 mm×100 mm,2.7μm),流动相为甲醇-5 mmol/L乙酸铵(含0.1%甲酸),梯度洗脱,流速为0.4 mL/min,柱温为40℃。采用电喷雾离子源正负离子同时扫描,多反应监测模式(MRM)进行质谱检测。结果:8种霉菌毒素在1.0～50.0 ng/mL范围内线性关系良好(R²>0.992),方法检出限在0.05～0.50μg/kg之间,定量限在0.17～1.65μg/kg之间;8种霉菌毒素加标回收率在75.6%～106.3%之间,相对标准偏差(RSD)为3.5%～9.3%。结论:该方法操作便捷、灵敏度高、准确可靠,能满足水产品中多种霉菌毒素残留快速检测需求。

Simultaneous Determination of 8 Mycotoxins in Aquatic Products by Liquid Chromatography-Tandem Mass Spectrometry Coupled with Immunoaffinity Column Clean-up

Objective: A liquid chromatography-tandem mass spectrometry coupled with immunoaffinity column clean-up method was established for the determination of 8 mycotoxins in aquatic products. Methods: The samples were extracted with acetonitrile water (84:16, V:V), and purified by multifunctional immunoaffinity columns. The chromatographic column was Agilent Proshell 120 SB·C₁₈ column (2.1 mm×100 mm, 2.7 μm). Mobile phase was methanol and 5 mmol/L ammonium acetate (containing 0.1% formic acid), gradient elution. The flow rate was 0.4 mL/min, and the column temperature was 40 ℃. The electrospray was operated in both positive and negative mode at the same time, and the samples were detected by multiple reaction monitoring mode (MRM). Results: The linear relations of the eight mycotoxins were good within the concentration range of 1.0~50.0 ng/mL (R2>0.992). The limits of detection were between 0.05~0.50 μg/kg, and the limits of quantification were between 0.17~1.65 μg/kg. The average recoveries were 75.6%~106.3%, and the relative standard deviations (RSDs) were 3.5%~9.3%. Conclusion: The method is simple, sensitive and accurate for the rapid analysis of mycotoxin residues in aquatic products.