超高效液相色谱－串联质谱法检测饲料中盐酸可乐定和盐酸赛庚啶

Determination of Clonidine hydrochloride and Cyproheptadine hydrochloride in Animal Feeds by Ultra Performance Liqμid Chromatography- Tandem Mass Spectrometry

关键词:  盐酸可乐定  盐酸赛庚啶  动物饲料  超高效液相色谱-串联质谱法

Key words:  Clonidine hydrochloride  Cyproheptadine hydrochloride  animal feeds  Ultra performance liquid chromatography-tandem mass spectrometry

摘要:

建立了检测饲料中盐酸可乐定和盐酸赛庚啶的超高效液相色谱-串联质谱（UPLC/MS/MS）分析方法。样品经酸性甲醇提取，浓缩后用乙腈-0.2%甲酸溶解，经超高效液相色谱-串联质谱在多反应检测（MRM）模式下测定。结果显示盐酸可乐定和盐酸赛庚啶标准曲线在0.2～50 μg/L浓度范围内线性良好。线性相关系数(r)分别为0.9994和0.9992；在0.02~1.0 mg/kg添加水平下，盐酸可乐定和盐酸赛庚啶的加标回收率在70～110%，相对标准偏差（RSD）均小于10%（n=6）；本方法对动物饲料中盐酸可乐定和盐酸赛庚啶的定量限为0.02 mg/kg (S/N＞10)，检出限为0.01 mg/kg (S/N＞3)。

Abstract:

A simple, sensitive and ultra performance liquid chromatography-tandem mass spectrometric (UPLC/MS/MS) method has been developed for the quantification of Clonidine hydrochloride and Cyproheptadine hydrochloride in animal feeds. Clonidine hydrochloride and Cyproheptadine hydrochloride extracted by methnol:0.1HCl（v/v,80/20）from animal feeds, was finally dissolved in acetonitrile:0.2%fomric acid（v/v,20/80）after the procedure of being concentration. The sample was separated on SB C18 (100mm?3.0mm i.d.,1.8 μm) column using a mobile phase of acetonitrile/0.2?. Clonidine hydrochloride and Cyproheptadine hydrochloride was detected in positive ion mode using multiple reactions monitoring (MRM). The quantitative analysis was finished in 6.0 min. Results showed that in the range of 0.2 to 50 μg/L the standard curves for Clonidine hydrochloride and Cyproheptadine hydrochloride were in good linearity , the correlation coefficients ( r) were 0. 9992 and 0.9994. The recoveries for Clonidine hydrochloride and Cyproheptadine hydrochloride at the addition of four levels (0.02~1.0 mg/kg) were 70% to 110% and the relative standard deviation (RSD) for the determination of chlorpromazine were less than 10% ( n = 6). The limits of quantity (S /N ≥10) and limits of detection(S /N ≥3) by the present method for Clonidine hydrochloride and Cyproheptadine hydrochloride were found to be 0.02 mg/kg and 0.01 mg/kg, respectively.