| 摘要: |
| 建立QuEChERS结合高效液相色谱-串联质谱测定乳粉中黄曲霉毒素B1(aflatoxin B1,AFB1)和黄曲霉毒素M1(aflatoxin M1,AFM1)的检测方法。方法 乳粉用水复溶,乙腈提取,十八烷基键合硅胶和无水硫酸镁净化,在InertSustain-C18柱(2.1 mm×150 mm,3μm)上分离,乙酸铵溶液-甲醇为流动相,梯度洗脱,电喷雾正离子模式扫描,多反应监测,基质添加外标曲线定量。结果 乳粉中AFB1和AFM在0.08~20 μg/kg浓度范围内线性关系良好,r＞0.999。检出限为AFM1 0.02 μg/kg,AFB1 0.03 μg/kg,定量限均为0.05 μg/kg。在定量限的1、5和10倍添加浓度下,平均回收率为91.5%~100.7%。结论 本方法便捷高效、重现性好、结果准确,可以为日常乳粉中黄曲霉毒素检测提供技术参考。 |
| 关键词: 乳粉 黄曲霉毒素B1和M1 QuEChERS 高效液相色谱-串联质谱法 |
| DOI： |
| 投稿时间：2022-05-28修订日期：2022-11-07 |
| 基金项目:“科技助力经济2020项目”(2020-032)；国家重点研发计划项目(2018YFC1603400)；中国检验检疫科学研究院基本科研业务费项目(2020 JK039) |
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| Determination of aflatoxin B1 and M1 in milk powder by QuEChERS-high performance liquid chromatography-tandem mass spectrometry |
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| (Hebei University of Engineering，Chinese Academy of Inspection and Quarantine) |
| Abstract: |
| A method for the determination of aflatoxin B1 and M1 in milk powder was established by QuEChERS combied with high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Milk powder was redissolved with water, extracted with acetonitrile, and the extract was purified by octadecyl bonded silica geland anhydrous magnesium sulfate. The samples were separated by InetSustain-C18 (2.1 mm×150 mm, 3μm)using ammonium acetate solution-methanol as mobile phase, and eluted in a gradient manner. Then detected by electrospray positive ion multiple and monitored by multiple reaction mode, and quantified by matrix-added external standard method. The concentrations of AFB1 and AFM1 in milk powder were in the range of 0.08-20 μg/kg, and the correlation coefficient(r) was higher than 0.999. The limit of detection were 0.02 μg/kg for AFM1 and 0.05 μg/kg for AFB1, and the limit of quantification were 0.05 μg/kg. At 1、5 and 10 times of the limit of quantitation, the average recoveries were 91.5%-100.7%. This method is convenient, efficient, reproducible and accurate, which can provide technical reference for daily detection of aflatoxin in milk powder. |
| Key words: milk powder aflatoxin B1 and M1 QuEChERS high performance liquid chromatography-tandem mass spectrometry |
