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目的采用亲水作用色谱-串联质谱检测技术和固相萃取前处理技术,建立动物源食品中氨丙啉残留量的检测方法。方法样品采用1%三氯乙酸-乙腈溶液(3∶7,V/V)提取,提取液经HLB小柱净化。以Se Quant ZICHILIC(150 mm×2.1 mm,5μm)色谱柱分离,含0.1%甲酸的5 mmol/L乙酸铵溶液-乙腈为流动相,40∶60(V/V)等度洗脱,电喷雾电离、正离子扫描、多反应监测模式测定,基质外标法定量。结果氨丙啉在0~500 ng/ml浓度范围内呈良好线性,相关系数大于0.999。定量限为10μg/kg。在鸡肉、鸡肝、鸡肾、鸡蛋、牛肉、牛肝、牛肾、牛奶和牛脂肪9种基质中加标回收率在73.2%~101.0%,相对偏差在2.09%~11.93%之内。结论该方法准确可靠、灵敏度高,适用于动物源食品中氨丙啉的定性定量分析。
Objective To establish a method for the determination of aminopropylamine residues in animal-derived foods by hydrophilic interaction chromatography-tandem mass spectrometry and solid-phase extraction pretreatment. Methods The samples were extracted with 1% trichloroacetic acid-acetonitrile (3: 7, V / V) and the extracts were purified by HLB cartridge. Separation was performed on a Se Quant ZICHILIC (150 mm × 2.1 mm, 5 μm) column with 5 mmol / L ammonium acetate in 0.1% formic acid in acetonitrile as mobile phase and 40:60 (V / V) Ionization, positive ion scan, multi-reaction monitoring mode determination, matrix external standard method. Results Aminopirline showed a good linearity in the range of 0-500 ng / ml with a correlation coefficient greater than 0.999. The limit of quantitation is 10 μg / kg. The spiked recoveries of nine substrates in chicken, chicken liver, chicken kidney, egg, beef, beef liver, beef kidney, milk and beef fat ranged from 73.2% to 101.0% with relative deviations within 2.09% ~ 11.93%. Conclusion The method is accurate and reliable and has high sensitivity. It is suitable for qualitative and quantitative analysis of Amprolium in animal-derived foods.