QuEChERS-高效液相色谱-串联质谱法测定乳粉中黄曲霉毒素B1和M1

Determination of aflatoxin B1 and M1 in milk powder by QuEChERS-high performance liquid chromatography-tandem mass spectrometry

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

Key words:  milk powder  aflatoxin B₁ and M₁  QuEChERS  high performance liquid chromatography-tandem mass spectrometry

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。

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.