乳业科学与技术 ›› 0, Vol. ›› Issue (): 0-0.

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PRiME MCX 固相萃取柱结合超高效液相色谱-串联质谱法测定乳和乳制品中25种β-受体激动剂药物残留

范力欣,范素芳,杨丽琼,任晓伟   

  1. 河北省食品检验研究院
  • 收稿日期:2024-06-06 修回日期:2024-08-09 出版日期:2024-05-01 发布日期:2024-08-26
  • 通讯作者: 范素芳

Determination of 25 β-receptor agonists drugs in milk and dairy products by PRiME MCX solid phase extraction column and ultra-performance liquid chromatography-tandem mass spectrometry

  • Received:2024-06-06 Revised:2024-08-09 Published:2024-05-01 Online:2024-08-26

摘要: 本研究基于超高效液相色谱-串联质谱技术,建立牛奶和乳制品中25 种β-受体激动剂的测定方法。样品经37℃酶解16h,0.2mol/L乙酸铵溶液(pH=5.2)提取,玻璃纤维滤纸除脂肪和蛋白质,PRIME MCX固相萃取柱净化,采用Waters BEH C18柱(100mm ×2.1mm,1.7μm)分离,以乙腈和0.1%甲酸水作为流动相进行梯度洗脱,采用电喷雾离子源,正离子多反应监测,内标法定量。结果表明:在0.2~50 ng/mL浓度范围内,25 种β-受体激动剂线性关系良好,相关系数(R2)大于0.996;回收率范围为80.3%~106.2%,相对标准偏差为0.7%~8.5%(n=6)。检出限范围为0.05~0.1 μg/kg;定量限范围为0.1~0.2 μg/kg。该方法简便高效,适用于牛奶和乳制品中25 种β-受体激动剂的测定。

关键词: 超高效液相色谱-串联质谱法, 牛奶, 奶制品, β-受体激动剂

Abstract: A method for the determination of 25 β-receptor agonists in milk and dairy products was established based on ultra-high performance liquid chromatography-tandem mass spectrometry.The samples were enzymolized in ammonium acetate solution for 16 h, fat and protein were removed by glass fiber filter paper,andpurified by PRIME MCX solid phase extraction column.The separation was performed using Waters BEH C18 column (100 mm ×2.1 mm, 1.7 μm). Acetonitrile and 0.1% formic acid water were used as mobile phase for gradient elution. Electrospray ion source was used, positive ion multiple reaction monitoring was performed, and quantitative determination was performed by internal standard method. The results showed that the linearity of the three vanillin analogues was good in the concentration range of 0.2~50ng/mL with the correlation coefficients (R2) greater than 0.996; the recoveries ranged from 80.3% to 106.2% with the relative standard deviations (RSDs) of 0.7%~8.5% (n=6). The method is simple, efficient and suitable for the determination of 25 β-receptor agonists in milk and dairy products.

Key words: ultra high performance liquid chromatography, milk, Dairy Product, β-receptor agonists