牛奶及乳粉中黄曲霉毒素M₁的液相色谱-质谱检测比较研究

目的：建立测定牛奶和乳粉中黄曲霉毒素M₁ 的液相色谱-质谱检测方法，并与国家标准方法比较。方法：采用ACQUITY UPLC HSS T3 色谱柱（50 mm×2.1 mm，1.8 μm），以0.1% 甲酸水溶液-乙腈为流动相进行梯度洗脱，流速0.3 mL·min^-1；采用电喷雾离子源进行正离子模式监测，多反应监测模式（MRM）定量分析，毛细管电压3.2 kV，离子源温度150 ℃ ；结果：在均满足日常检测的情况下，本方法较国家标准方法回收率提高10% 以上，检出值准确性提高5% 以上。测定结果显示采集的市售牛奶和乳粉中均未检出黄曲霉毒素M₁，牛奶质控样品（3.03±0.70）μg·kg^-1 测定结果为（3.05±0.08）μg·kg^-1（n=5），乳粉阳性样品（1.00±0.25）μg·kg^-1 测定结果为（1.10±0.02）μg·kg^-1（n=5）。结论：牛奶及乳粉中黄曲霉毒素M₁ 的检测可以通过简单制备后进行测定，为日常检测提供了简便可行的方法。

Objective: To develop a method for the determination of alfatoxin M₁ in milk and its powder,and to compare it with current national standard method. Methods: The samples were separated on a nACQUITY UPLC HSS T3 column(50 mm×2.1 mm,1.8 μm)with a mobile phase of acetonitrile and water containing 0.1% formic acid in a gradient elution at a flow rate of 0.3 mL·min^-1. Multiple-reaction monitoring(MRM)scanning was employed for quantification with switching electrospray ion source polarity in positive mode. The capillary voltage was set at 3.2 kV,and the ion source temperature was maintained at 150℃. Results: Both methods could cope with routine test, while the new developed method had by 10% higher recovery rate than the standard method,and the accuracy of target results was promoted by 5%. Aflatoxin M₁ was not detected in both commercially available milk and milk powder, while the results of the determination of quality controled samples in milk with(3.05±0.08)μg·kg^-1(n=5), and in milk powder with(1.10±0.02)μg·kg^-1(n=5)were(3.03±0.70)μg·kg^-1and(1.00±0.25)μg·kg^-1,respectively. Conclusion: Alfatoxin M₁ in milk and its powder could be determined after simple treatment and the method provided a simple and easy way for routine tests.

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