液质联用法检测知柏地黄丸中氯霉素残留的研究

Study on determination of chloramphenicol residue in Zhibai Dihuang pills by liquid chromatography tandem mass spectrometry

目的:建立高效液相色谱串联质谱技术测定知柏地黄丸中残留氯霉素的含量。方法:采用高效液相-电喷雾-串联四极杆质谱法(HPLC-ESI--MS-MS)测定知柏地黄丸中残留氯霉素的含量。选用Thermo C18(250 mm×4.6 mm,5μm)色谱柱,流动相为甲醇-水(起始比例为40∶60,梯度洗脱),流速为0.5 mL·min-1,进样量为20μL,定量离子对为m/z 152(负离子),监测模式为多重反应监测(MRM)。结果:测定的检出限为0.2μg·kg-1,线性范围为1.0～200 ng·mL-1,回收率为87.64%～94.23%,RSD为1.7%～13%。结论:该方法操作简便、灵敏、准确,能够满足残留检测的要求。

To establish a method for determination of chloramphenicol residue in Zhibai Dihuang pills by high performance liquid chromatography tandem mass spectrometry. Methods： Chloramphenicol residue in Zhibai Dihuang pills was determined by high performance liquid chromatography tandem mass spectrometry. The a- nalysis was carried on a Thermo Cis column （250 mm × 4.6 mm,5 μm）. The mobile phase was composed of metha- nol and water （initial proportion 40： 60, gradient） ; the flow rate was 0.5 mL · min- l and the injection volume was 20μL; the quantitation ion was m/z 152 （the negative ionization） under the mode of multiple reaction monitoring. Results ： The limit of detection （LOD） was 0.2 μg · kg- 1 and the linear range was between 1.0 ng · mL- 1 and 200.0 ng · mL-1 ,the average recovery of choramphenicol was between 87.64% and 94. 23% with RSD values between 1.7% and 13%. Conclusion： The method is convenient, sensitive and accurate,which meets the require- ments for residue determination.