College of Agriculture and Biology, Shanghai Jiao Tong University, Shanghai, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Apr 1;879(11-12):799-803. doi: 10.1016/j.jchromb.2011.02.030. Epub 2011 Feb 25.
A simple and sensitive analytical method was developed for the simultaneous determination of clenbuterol, chloramphenicol and diethylstilbestrol in bovine milk by isotope dilution ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Samples were directly purified through HLB cartridge. The organic phase was dried under nitrogen and residues were redissolved in mobile phase. Samples were analyzed by UPLC-MS/MS on an Acquity UPLC® BEH C(18) column with gradient elution. The samples were quantified using clenbuterol-D(9), chloramphenicol-D(5) and diethylstilbestrol-D(8) as internal standards. The proposed method was validated according to the European Union regulation 2002/657/EC determining specificity, decision limit (CCα), detection capability (CCβ), trueness, precision, linearity and stability. The method is demonstrated to be suitable for the determination of clenbuterol, chloramphenicol and diethylstilbestrol in bovine milk. The total time required for the analysis of one sample was about 50min.
建立了一种超高效液相色谱串联质谱法（UPLC-MS/MS），用于同时测定牛奶中克伦特罗、氯霉素和己烯雌酚。样品直接通过 HLB 小柱净化，有机相氮气吹干后用流动相重溶。样品在 Acquity UPLC® BEH C(18)柱上进行 UPLC-MS/MS 分析，采用梯度洗脱。使用克伦特罗-D(9)、氯霉素-D(5)和己烯雌酚-D(8)作为内标进行定量。该方法按照欧盟 2002/657/EC 法规进行验证，包括特异性、决策限（CCα）、检测能力（CCβ）、准确度、精密度、线性和稳定性。该方法适用于牛奶中克伦特罗、氯霉素和己烯雌酚的测定。分析一个样品的总时间约为 50min。
