HPLC-MS/MS法快速测定乳制品中90种兽药的残留量

目的 建立高效液相色谱-串联质谱法（HPLC-MS/MS）测定乳制品中十大类90种兽药残留的检测方法。方法 试样用0.2%甲酸乙腈溶液提取，经Waters Prime HLB固相萃取柱净化，用Waters XBridge BEH-C18色谱柱洗脱分离，并使用电喷雾电离源，正负离子切换扫描模式进行检测，外标法定量。结果90种兽药在1 ng/mL～20 ng/mL范围内呈现良好的线性相关性，相关系数均大于0.995。90种兽药的方法检出限为0.3 ?g/kg，方法定量限为1 ?g/kg。在添加量为1 ?g/kg、2 ?g/kg和10 ?g/kg的加标回收实验下，90种兽药的加标回收率范围分别为66.0%～134.8%，64.0%～122.4%和62.4%～118.3%。同时做了方法精密度验证，有69%的兽药RSD<5%，有28%的兽药RSD在5%～10%，有3%的兽药RSD在10%～20%。结论 该方法简单、快速、高效且能同时准确定性和定量检测乳制品中十大类90种兽药的残留量。

Rapid determination of 90 veterinary drug residues in dairy products by high performance liquid chromatography-tandem mass spectrometry

Objective To establish a method for determination of ten categories of 90 veterinary drug residues in dairy products by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were extracted with 0.2% formic acid-acetonitrile solution, and then purged by Waters Prime HLB solid phase extraction column. The extracts was eluted and separated by the Waters XBridge BEH-C18 chromatographic column, and the electrospray ionization source was used and the positive and negative ion switching mode was used to detect it. Results The 90 kinds of veterinary drugs showed good linear correlation in the range of 1 ng/mL~20 ng/mL, and the correlation coefficient was more than 0.995. The LODs and LOQs of 90 kinds of veterinary drugs were 0.3 ?g/kg and 1 ?g/kg. Under the additive recovery experiment of 1 ?g/kg, 2 ?g/kg and 10 ?g/kg, the recovery rates of the 90 kinds of veterinary drugs were 66%~134.8%, 64%~122.4% and 62.4%~118.3%, respectively. The accuracy of the method was verified. The relative standard deviation of 69% veterinary drugs is less than 5%, the relative standard deviation of 28% veterinary drugs is 5% to 10%, and the relative standard deviation of only 3% of the veterinary drugs is 10% to 20%. Conclusion The method is simple, rapid, efficient and can be used to determine and quantify the residues of ten categories of 90 kinds of veterinary drugs in dairy products at the same time.