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Journal of Dairy Science and Technology ›› 2018, Vol. 41 ›› Issue (4): 29-33.DOI: 10.15922/j.cnki.jdst.2018.04.007

• Analysis & Detection • Previous Articles     Next Articles

Quantitative Determination of Cephalosporin Residues in Dairy Products by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with PRIME HLB Solid Phase Extraction

MO Nan, ZHANG Lijia, Lü Zhiyong, DUAN Guoxia, LIU Lijun, LI Cuizhi, ZHAO Jing, HU Xue   

  1. (Inner Mongolia Yili Industrial Group Co. Ltd., Hohhot 010110, China)
  • Online:2018-07-01 Published:2021-11-18

PRIME HLB固相萃取/超高效液相色谱-串联质谱法测定乳制品中头孢菌素类药物残留

莫楠张立佳吕志勇段国霞刘丽君李翠枝赵静胡雪   

  1. 内蒙古伊利实业集团股份有限公司,内蒙古 呼和浩特,010110

Abstract: An ultra performance liquid chromatography-tandem mass spectrometry method for the simultaneous quantitative determination of four cephalosporin residues in dairy products, including milk, yogurt and milk powder, has been established. The samples were extracted with 5% formic acid acetonitrile. After being purified by solid-phase microextraction using an Oasis PRIME HLB cartridge, the extract was blown to dryness under a stream of nitrogen gas and then re-dissolved. The analysis was carried out using a positive electrospray ion source in the multiple reaction monitoring mode. The limit of quantification was 32 μg/kg for cefalexin, cefapirin, cefalonium and cefquinome?in milk powder; the limit of quantification was 4 μg/kg in milk and yogurt. The recoveries at spiked concentration levels of 4-150 μg/kg were 63.3%-112.1%, with relative standard deviations of 1.6%-10.5%. The matrix effects were 108.77%-379.91%. This method was characterized by short analysis time and was suitable for the determination of cephalosporin residues in different dairy products.

Key words: ultra performance liquid chromatography-tandem mass spectrometry; cephalosporin; veterinary residues; dairy products; Oasis PRIME HLB catridge

摘要: 建立牛乳、酸乳和乳粉3 种基质乳制品中采用超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时检测4 种头孢菌素类药物残留的方法。以5%甲酸乙腈溶液进行提取,经Oasis PRIME HLB固相萃取柱净化,氮吹后复溶,采用电喷雾离子源正离子模式及多反应监测模式进行检测。结果表明:牛乳和酸乳中头孢氨苄、头孢匹林、头孢洛宁和头孢喹肟的定量限为4 μg/kg,乳粉中为32 μg/kg

关键词: 超高效液相色谱-串联质谱;头孢菌素类;兽药残留;乳制品;Oasis PRIME HLB固相萃取柱

CLC Number: 

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