超高效液相色谱-串联质谱测定白酒中的黄曲霉毒素B1B2G1G2总量

Simultaneous detection of aflatoxin total B1B2G1G2 in Chinese liquor by ultra high performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高相液相色谱—串联质谱仪  黄曲霉毒素总量  白酒

英文关键词:ultra high performance liquid chromatography-tandem mass spectrometry  aflatoxin total  Chinese liquor

中文摘要:

      目的 建立一种超高效液相色谱—串联质谱(ultra-high performance liquid chromatography-tandem mass spectrometry, UPLC-MS)测定白酒中黄曲霉毒素总量(G2, G1, B2, B1)的检测方法。方法 以甲醇+5 mmol/L乙酸铵作为流动相梯度洗脱, 流速为0.2 mL/min, 经ACQUITY UPLC BEH C18(50 mm×2.1 mm, 1.7 μm)色谱柱, 柱温为40 ℃, 采用电喷雾电离源正离子模式检测, 进样时间为10 min。结果 经检测, 黄曲霉毒素总量均有较好的线性关系, 线性相关系数r2均大于0.999。检出限在0.01~0.03 μg/kg之间。加标回收率为87~103%。结论 用所建方法同GB 5009.22-2016从时间、样品处理及最后结果上进行对比分析, 该方法简单、快速, 结果准确, 灵敏度高。

英文摘要:

      Objective To establish a method for simultaneous detection of aflatoxin total (AFT) (G2, G1, B2 and B1) by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS) in Chinese liquor. Methods A gradient elution program of methanol-5 mmol/L ammonium acetate as mobile phase was adopted at the flow rate of 0.2 mL/min, ACQUITY UPLC BEH C18(50 mm×2.1 mm, 1.7 μm) chromatographic column was adopted. The column temperature was maintained at 40 ℃. By using electrospray ionization source in positive ion mode with the injection time as 10 min. Results Aflatoxin total had a good linear relationship in their individual linear ranges, and the linear correlation coefficient r2 was above 0.999. The detection limit was between 0.01 μg/kg to 0.03 μg/kg. The spiked recovery rate were 87% to 103%. Conclusion The method is compared with the standard GB 5009.22-2016 to analyze the time, sample processing and final results. The method was simple, rapid, accurate, and sensitive.