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目的:建立测定牛奶和乳粉中黄曲霉毒素M_1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,1.8μm),以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,流速0.3mL·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 k V,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M_1,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M_1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 establish a liquid chromatography - mass spectrometry method for the determination of aflatoxin M_1 in milk and milk powder and to compare with the national standard method. METHODS: The gradient elution was performed on a ACQUITY UPLC HSS T3 column (50 mm × 2.1 mm, 1.8 μm) using 0.1% formic acid in acetonitrile as the mobile phase at a flow rate of 0.3 mL · min -1. Electrospray ionization Source for positive ion mode monitoring, multiple reaction monitoring mode (MRM) quantitative analysis, capillary voltage 3.2 kV, ion source temperature 150 ℃; Results: In the case of meet the daily test, the method than the national standard method to improve the recovery rate of 10 % Or more, the detection accuracy of 5% or more. The results showed that aflatoxin M_1 was not detected in commercially available milk and milk powder, and 3.03 ± 0.70 μg · kg -1 in milk was (3.05 ± 0.08) μg · kg ~ (-1) (-1) (n = 5). The results of (1.00 ± 0.25) μg · kg -1 of the milk powder positive sample were (1.10 ± 0.02) μg · kg -1 (n = 5). Conclusion: The determination of aflatoxin M 1 in milk and milk powder can be determined by simple preparation and provides a simple and feasible method for routine testing.