液质联用法检测知柏地黄丸中氯霉素残留的研究

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，5 μm)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20 μL，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0.2 μg·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。

Objective: 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 analysis was carried on a Thermo C₁₈ column (250 mm×4.6 mm,5 μm).The mobile phase was composed of methanol and water (initial proportion 40∶60,gradient); the flow rate was 0.5 mL·min^-1 and the injection volume was 20 μL; 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 requirements for residue determination.

1 ChP(中国药典)[S].2010.VolⅠ(一部):820
2 FENG Feng(冯峰).Reason of excessive antibiotic residues in honey and its control countermeasures (蜂蜜中抗生素残留超标的原因剖析及其控制对策)[J].Bees Mag (蜜蜂杂志),2002,10(1):23
3 XIE Shou-xin(谢守新),LIN Hai-dan(林海丹),QIN Yan(秦燕),et al.Determination of chloramphenicol in aquatic products with internal standard by liquid chromatography coupled to electrospray ionization tandem mass spectrometry (液相色谱-电喷雾串联质谱内标法测定水产品中氯霉素药物残留) [J].Chin J Health Lab Technol(中国卫生检验杂志),2006,16(11):1298
4 YUE Zhen-feng(岳振峰),CHEN Xiao-xia(陈小霞),ZHENG Wei-ping(郑卫平),et al.A study on the LC-ESI-MS-MS analysis of chloramphenicol in chicken (高效液相色谱-电喷雾三级四极杆质谱测定鸡肉组织中氯霉素残留的研究) [J].J Instrum Anal (分析测试学报),2005,24(1):80
5 CHEN Xiao-xia(陈小霞),YUE Zhen-feng(岳振峰),JI Cai-ni(吉彩霓),et al.Analysis of chloramphenicol,thiamphenicol and florfenicol in chickens by high performance liquid chromatography with electrospray ionization mass spectrometry (高效液相色谱-电喷雾电离三级四极杆质谱测定鸡肉中氯霉素、甲砜霉素和氟甲砜霉素的残留量) [J].Chin J Chromatogr (色谱),2005,23(1):92
6 JI Wen-liang(吉文亮),MA Yong-jian(马永建),CANG Gong'ao(仓公敖).Quantity of chloramphenicol in honey by liquid chromatography coupled with electrospray ionization tandem mass spectrometry (高效液相色谱串联质谱法测定蜂蜜中残留氯霉素) [J].Chin J Pharm Anal(药物分析杂志),2006,26(12):1814
7 Blomgren A,Berggren C,Holmberg A,.Extraction of clenbuterol from calf urine using a molecularly imprinted polymer followed by quantitation by high-performance liquid chromatography with UV detection[J].J Chromatogr A, 2002,975(1):157
8 Theodoridis G,Manesiotis P.Selective solid-phase extraction sorbent for caffeine made by molecular imprinting[J].J Chromatogr A,2002,948(1-2) :163
9 Shi X,Wu A,Zheng S,et al.Molecularly imprinted polymer microspheres for solid-phase extraction of chloramphenicol residues in foods[J].J Chromatogr B,2007,850(1-2):24
10 Andersson LI.Molecular imprinting for drug bioanalysis:A review on the application of imprinted polymers to solid-phase extraction and binding assay[J].J Chromatogr B,2000,739(1) :163
11 Wulff G,Sarhan A,Zabrocki K.Enzyme analogue built polymers and their use for the resolution of racemates[J].Tetrahedron Lett,1973:4329
12 ZHOU Qin(周卿),PU Jia-zhi(蒲家志).Molecular imprinting technology in the separation of drugs (分子印迹技术在药物分离中的应用)[J].Zunyi Med Coll(遵义医学院学报),2004,27( 6):597