| 摘要: |
| 本研究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0.1mol/L NaOH溶解后,用0.1mol/L HCl溶液调节pH值至7.0,经乙腈提取后用LC-MS/MS进行分析。分析时采用Waters BEH C18色谱柱(100mm×2.1mm,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,样品中添标回收率在85%～110%之间,相对标准偏差(RSD)小于10%。 |
| 关键词: 高效液相色谱-串联质谱 盐酸可乐定 盐酸赛庚啶 猪毛 |
| DOI： |
| 投稿时间：2015-05-13修订日期：2015-07-03 |
| 基金项目:宁波市农科教项目(2014NK36) |
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| Determination of Clonidine Hydrochloride and CyproheptadineHydrochloride in Swine Hair by Ultra Performance Liquid Chromatography -Tandem Mass Spectrometry |
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| (Ningbo Academy of Agricultural Sciences) |
| Abstract: |
| A simple and sensitive LC-MS/MS method for the determination of Clonidine Hydrochloride and Cyproheptadine Hydrochloride in swine hair was developed. Samples were dissolved with 0.1mol/L NaOH, adjusted the pH value to 7.0 by 0.1mol/L HCl, extracted with acetonitrile and analyzed by LC/MS-MS on a Waters Acquity BEH C18 column with 0.10% formic acid in water/methanol as the mobile phase by means of gradient elution. Detection was carried out with an electrospray ionisation (ESI) probe and operated in the positive ion mode. Clonidine Hydrochloride and Cyproheptadine Hydrochloride was quantified by the external standard method. There was a good linearity in the range of concentrations between 1.0 and 50.0 μg/L. The limits of detection for Clonidine Hydrochloride and Cyproheptadine Hydrochloride were both 0.2μg/L. The recoveries from spiked samples were in the range of 85% to 110% and the relative standard deviations were lower than 10%. |
| Key words: ultra performance liquid Chromatography-Tandem Mass Spectrometry clonidine hydrochloride cyproheptadine hydrochloride swine hair |
