摘要
目的建立超高效液相色谱-串联质谱法（UPLC-MS/MS）同时测定鸡肉、鸡蛋中氯霉素（CAP）和甲硝唑（MNZ）的检测方法。方法以氘代氯霉素（D5-CAP）和氘代甲硝唑（D4-MNZ）为内标,样品采用乙酸乙酯提取,氮气吹干后用0.1 mol/L HCl复溶,正己烷脱脂,MCS固相萃取柱净化处理。在ACQUITY BEH-C18色谱柱中分离,以0.05%氨水-乙腈做流动相,梯度洗脱,氯霉素采用ESI-监测模式、甲硝唑采用ESI＋监测模式,均采用同位素内标法定量。结果鸡肉、鸡蛋样品中氯霉素和甲硝唑的检出限均为0.01μg/kg;氯霉素的回收率为101.4%~104.3%,相对标准偏差为3.0%~9.1%;甲硝唑的回收率为101.0%~104.9%,相对标准偏差为4.4%~8.8%。结论本法具有良好的选择性、灵敏度和准确度,满足鸡肉、鸡蛋样品中痕量氯霉素、甲硝唑药物残留的高灵敏分析。
Objective To develop a method for the simultaneous detection of chloramphenicol and metronidazole in chicken and eggs by ultra- performance liquid chromatography tandem mass spectrometry（ UPLC- MS / MS）. Methods Coupled with internal standards of D5- chloramphenicol and D4- metronidazole,samples were extracted with ethyl acetate. The extraction was dried under nitrogen and then redissolved with 0. 1 mol / L HCl,defatted with n- hexane,cleaned- up with MCS solid phase column. CAP and MNZ were separated by gradient elution with 0. 05% ammonia water- acetonitrile in ACQUITY BEH- C18 column. CAP and MNZ were quantified by isotope internal standard method respectively in ESI-mode and ESI＋mode.Results The limits of detection for CAP and MNZ in chicken and eggs were 0. 01 μg / kg. The spiking average recoveries for CAP and MNZ in chicken were within 101. 4%- 104. 3% and 101. 0%- 104. 9%,respectively,and the relative standard deviation（ RSDs） of them were within 3. 0%- 9. 1% and 4. 4%- 8. 8%,respectively. Conclusion The method was selective,sensitive,accurate and suitable for the analysis of trace CAP and MNZ in chicken and eggs.
出处
《中国卫生检验杂志》
CAS
2016年第21期3083-3085,3097,共4页
Chinese Journal of Health Laboratory Technology
基金
国家青年科学基金项目(31501565)
关键词
超高效液相色谱-串联质谱
氯霉素
甲硝唑
抗生素残留
Ultra-performance liquid chromatography tandem mass spectrum
Chloramphenicol
Metronidazole
Antibiotics residues
