高效液相色谱-串联质谱法同时定性和定量检测牛奶中106种兽药残留

Simultaneous qualitative and quantitative determination of 106 kinds of veterinary drug residues in milk by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  牛奶  多兽药残留  定性  定量  高效液相色谱-串联质谱法

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

中文摘要:

      目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)同时定性和定量检测牛奶中106种兽药残留的分析方法。方法 牛奶中的兽药经甲酸化乙腈提取后, 加入硫酸钠、氯化钠、二水柠檬酸三钠和柠檬酸氢二钠进行液-液分配, 离心后上清液经C18, 氮丙级乙二胺(primary secondary amine, PSA)和硫酸钠混合的分散式固相萃取填料(dispersive solid phase extraction, d-SPE)净化, 然后经过HPLC-MS/MS进样和采集数据。结果 在当前验证的目标筛查浓度(screening target concentration, STC)下, 100种兽药通过了定性方法验证, 假阳性率和假阴性率都小于5%; 74种兽药通过了定量方法验证, 回收率满足70%~120%的要求, 重现性标准偏差不大于20%。结论 此方法适用于牛奶中多兽药的同时定性和定量检测, 可以应用于日常检测及合规性的判定。

英文摘要:

      Objective To establish an analytical method for the simultaneous qualitative and quantitative detection of 106 veterinary drug residues in milk by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods Veterinary drug residues in milk were extracted with a mixture of formic acid and acetonitrile followed by a liquid-liquid partition using sodium sulphate, sodium chloride and citrate salts. After centrifugation, supernatant was cleaned by dispersive solid phase extraction (d-SPE) which consists of a mixture of sodium sulphate, primary secondary amine (PSA) and C18 sorbents. Results At current screening targeted concentration (STC), the 100 kinds of veterinary drug residues passed through the qualification validation criteria, with false positive and negative rate were both less than 5%; the 74 kinds of veterinary drug passed through the quantification validation criteria, with recovery rate met 70%–120% requirement and standard deviation of reproducibility was less than 20%. Conclusion The developed method can be applied for qualification and quantification of multi-veterinary drug residues in milk, and it also can be used for routine analysis and compliance check.