高效液相色谱-串联质谱法测定猪毛中盐酸可乐定和盐酸赛庚啶

Determination of Clonidine Hydrochloride and Cyproheptadine Hydrochloride in Swine Hair by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了高效液相色谱-串联质谱法测定猪毛中盐酸可乐定和盐酸赛庚啶的方法。猪毛样品用0.1 mol/L NaOH溶解后,用0.1 mol/L HCl溶液调节pH值至7.0,经乙腈提取后用UPLCMS/MS进行分析。分析时采用Waters BEH C18色谱柱(100 mm×2.1 mm,1.7μm),以0.10%甲酸水/甲醇作为流动相进行梯度洗脱,电喷雾正电子(ESI^+)模式电离,多反应监测(MRM)模式检测,外标法进行定量。结果表明:盐酸可乐定和盐酸赛庚啶标准溶液在1.0~50μg/L范围内,峰面积与含量呈线性相关。盐酸可乐定和盐酸赛庚啶的检出限均为0.20μg/kg,样品中添标平均回收率在85%~110%之间,相对标准偏差(RSD)小于10%。

A simple and sensitive UPLC - MS/MS method for the determination of clonidinehydrochloride andeyproheptadine hydrochloride in swine hair was developed. Samples were dissolved with 0. lmol/L NaOH, adjusted the pH value to 7.0 by 0.1 mol/L HCl, extracted with acetonitrileand analyzed by UPLC/MS - MS on a WatersAcquity BEH C18 column with 0. 10% formic acid in water/methanol as the mobile phase by means of gradient elution. Detection wascarried out with an eleetrospray ionisation （ESI） probe and operated in the positive ion mode. Clonidinehydrochloride andcyproheptadine hydrochloride was quantified by the externalstandard method. There was a good linearity in the range of concentrations between 1.0 and 50.0 μg/L. The limits of detection forclonidinehydroehloride andcyproheptadine hydrochloride were both 0.2 μg/L. The average recoveries from spiked samples were in therange of from 85% to 110% and the relative standard deviations were lower than 10%.