高效液相色谱-串联质谱法同时检测畜产品中67种兽药残留

Simultaneous determination of 67 kinds of veterinary drug residues in livestock products by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  畜产品  兽药残留

英文关键词:high performance liquid chromatography-tandem mass spectrometry  livestock products  veterinary drug residues

中文摘要:

      目的 建立一种基于猪肉、牛肉、羊肉为基质的高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)同时检测磺胺类、喹诺酮类、苯并咪唑类、β受体激动剂类、四环素类、糖皮质激素类、硝基咪唑类、大环内脂类、酰胺醇类等9大类67种兽药残留。方法 样品经0.1 mol/L乙二胺四乙酸二钠(ethylenediaminetetraacetic acid disodium salt, EDTA-2Na)水溶液预处理后用0.2%甲酸乙腈提取, 通过PRiME HLB固相萃取柱净化, 40℃氮气浓缩后90%水-乙腈溶液(含0.05%甲酸)溶液复溶, InfinityLab Proroshell 120 EC-C18色谱柱分离, 以AJS ESI离子源在正、负离子多反应监测模式下进行测定。结果 67种兽药经0.1 mol/L EDTA-2Na水溶液(含0.2%甲酸)-乙腈(8:2, V:V)提取后, 在1~50 μg/L的质量浓度范围内线性关系良好, 相关系数r2均大于0.999, 67种化合物的检出限(limits of detection, LODs)为0.02~1.35 μg/kg, 定量限(limits of quantification, LOQs)为0.05~4.51 μg/kg; 在加标水平为5、10、50 μg/kg时, 回收率为61.6%~112.7%, 相对标准偏差(relative standard deviations, RSDs)为1.0%~15.3%。结论 该方法前处理过程简单、试剂用量小、检测灵敏、准确度高, 极大提高了风险监测检测效率, 将在各级大范围初级畜禽产品风险监测项目的初步筛查工作中发挥重要作用。

英文摘要:

      Objective To establish a method for the simultaneous determination of 67 kinds of veterinary drug residues in 9 categories including sulfonamides, quinolones, benzimidazoles, β-agonists, tetracyclines, glucocorticoids, nitroimidazoles, macrolides and amide alcohols based on pork, beef and mutton by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were pretreated with 0.1 mol/L ethylenediaminetetraacetic acid disodium salt (EDTA-2Na) aqueous solution, extracted with 0.2% formic acid acetonitrile, purified by PRiME HLB solid phase extraction column, concentrated by nitrogen at 40℃, redissolved with 90% water-acetonitrile solution (containing 0.05% formic acid) solution, separated by InfinityLab Proroshell 120 EC-C18 chromatographic column, and determined by AJS ESI ion source in positive and negative ion multi-reaction monitoring mode. Results The 67 kinds of veterinary drugs were extracted by 0.1 mol/L EDTA-2Na aqueous solution (containing 0.2% formic acid)-acetonitrile (8:2, V:V). The linear relationship was good in the mass concentration range of 1–50 μg/L, and the correlation coefficient r2 was greater than 0.999. The limits of detection (LODs) range of 67 kinds of compounds were 0.02–1.35 μg/kg, and the limits of quantification (LOQs) range were 0.05–4.51 μg/kg. When the spiked levels were 5, 10, 50 μg/kg, the recoveries were 61.6%–112.7%, and the relative standard deviations (RSDs) were 1.0%–15.3%. Conclusion The method has the advantages of simple pretreatment process, small reagent dosage, high sensitivity and accuracy, which greatly improves the efficiency of risk monitoring and detection. It will play an important role in the preliminary screening of risk monitoring projects of large-scale primary livestock and poultry products at all levels.