高效液相色谱-高分辨质谱法定性筛查牛奶中49种β-内酰胺类抗生素残留

目的 开发和验证定性筛查牛奶中49种β-内酰胺类抗生素残留的高效液相色谱-高分辨质谱法(high performance liquid chromatography coupled with high resolution mass spectrometry,HPLC-HRMS)。方法牛奶经磷酸盐缓冲液及乙腈提取后,加入硫酸钠(Na2SO4)和氯化钠(NaCl)进行盐析,离心后取部分上清液经Na2SO4和C18混合的分散式固相萃取填料(dispersive solid phase extraction,d-SPE)净化,净化液浓缩定容后,使用HPLC-HRMS分别以全扫描-数据依赖型二级扫描(full scan-data dependent secondary acquisition,Full MS/dd-MS2)和全扫描-平行反应监测二级扫描(full scan-selected ion monitoring/parallel reaction monitoring,Full MS/PRM)两种模式进行数据采集。结果在Full MS/PRM模式下,45种抗生素通过方法验证,假阳性率和...

Qualitative screening of beta-lactam antibiotic residue in milk by high performance liquid chromatography coupled with high resolution mass spectrometry

Objective To developed and validate a targeted screening method for determination of 49 kinds of beta-lactam antibiotic residues in milk by high performance liquid chromatography coupled with high resolution mass spectrometry (HPLC-HRMS). Method Milk was extracted with a mixture of a phosphate buffer solution and acetonitrile followed by a salt partition using sodium sulphate (Na2SO4) and sodium chloride (NaCl). After centrifugation, an aliquot of the supernatant was cleaned by dispersive Solid Phase Extraction (d-SPE) which consisted of a mixture of Na2SO4 and octadecyl-silica C18 sorbents. Result The resulting extract was then concentrated before injection into LC-HRMS, data acquired by two scanning modes (Full MS/dd-MS2& Full MS/PRM). At the Full MS/PRM mode, 45 kinds of drug residues passed through the validation with false positive and negative rate are less than 5%; At Full MS/dd-MS2 mode, 43 kinds of antibiotics passed through the validation with false positive and negative rate are less than 5%. Conclusion The research showed that the method could be applied for qualitative determination of beta-lactam antibiotics residues in milk. Comparing to Full MS/dd-MS2, Full MS/PRM was more robust, and it was suitable for targeted screening of veterinary drug residues in complex matrix