UPLC-MS定性定量检测中成药中非法添加的盐酸克仑特罗

Qualitative and Quantitative Determination of Clenbuterol Hydrochloride in Chinese Patent Medicines by UPLC-MS

目的:建立UPLC-MS方法,快速定性定量检测中成药中非法添加的盐酸克仑特罗。方法:采用超高效液相色谱串联三重四极杆质谱仪。色谱条件:Agela Venusil MP-C18色谱柱(2.1 mm×50 mm,3μm),柱温35℃,流动相甲醇-0.2%甲酸水溶液(50∶50),流速0.3 mL.min-1。质谱条件:ESI源,多反应检测(MRM)。以保留时间及定性离子对之间的相对丰度定性,以定量离子对峰面积定量。结果:盐酸克仑特罗在1.092～27.300μg.L-1呈现良好的线性关系(r>0.999 8);平均加样回收率97.26%;定量限为0.19 pg。结论:本方法定性可靠、定量准确,且快速简便,可用于中成药非法添加盐酸克仑特罗化学药品的检测。

Objective： To establish an UPLC-MS method for determination of Clenbuterol hydrochloride in Chinese patent medicines. Method： Ultra performance liquid chromatography tandem three quadrupole mass spectrometer was adopted, LC condition： A agela Venusil MP-C18 （2.1 mm ×50 mm, 3 μm） column was used with the isocrstic elution of methanol and 0.2% methanoic acid at a flow rate 0. 3 mL ·min^-1 MS condition： adopted electrospray ionization （ESI）, and multiple reaction monitoring, The relative intensities of the detected qualitative ion pairs using for qualitative, integrating the signals of the detected quantitative ion pairs using for quantitative. Result： The clenbuterol hydrochloride had good linearity with correlation coefficient 〉 0. 999 8, ranging from 1. 092-27. 300 μg·L^-1. The average recoveries were 97.26%. The limit of quantitation was 0. 19 pg. Conclusion： This method is reliable qualitative and quantitative accuracy, simple and rapid, and can be used for proprietary Chinese medicines illegally added clenbuterol hydrochloride detection.