UPLC-MS/MS检测原料奶中脱呋喃甲酰基头孢噻呋残留方法的建立
Establishment on UPLC-MS/MS detection methods for desfuroylceftiofur in raw milk
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摘要: 目的:建立超高压液相色谱-串联质谱法（UPLC-MS/MS）测定原料奶中脱呋喃甲酰基头孢噻呋来间接衡量头孢噻呋残留的方法。方法:利用T3色谱柱,以含有0.02%的甲酸水-乙腈溶液为流动相进行梯度洗脱,采用二硫赤藓糖醇将原料奶中头孢噻呋分解为脱呋喃甲酰头孢噻呋（DFC）,由碘乙酰胺衍生化为稳定的DFC乙酰胺形式（DCA）,样品再经HLB固相萃取柱富集净化后,进行UPLC-MS/MS检测。结果:m/z 430.12>125.79为定量离子对,m/z 430.12>241.04为定性离子对,回收率在98.6%102.2%,精密度（RSD）为2.51%3.87%,最低检出限为0.45ng/mL。结论:该方法可用于原料奶中脱呋喃甲酰基头孢噻呋残留的测定。Abstract: Objective:A ultra-high pressure liquid chromatograph-tandem mass spectrometry (UPLC-MS/MS) was established for determination of desfuroylceftiofur residues in raw milk. Methods:T3 column was used with a mixed solution of 0.02% formic acid-acetonitrile as mobile phase. The cefliofur in bovine raw milk was decomposed by dithioerythritol to produce desfuroylceftiofur (DFC) , which was further stabilized by derivatization to desfuroylceftiofur acetamide (DCA) using iodoacetamide, then the samples were concentrated and purified by HLB SPE cartridge and determined by UPLC-MS/MS.Results:The quantitative ion was m/z 430.12>125.79.The qualitative ion was m/z 430.12>241.04. The recovery were 98.6%~102.2%, the relative standard deviations (RSD) were 2.51%~3.87%, the minimum detectable values were 0.45ng/mL. Conclusion:This method could be used for the routine analysis of desfuroylceftiofur residues in raw milk.
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