超高效液相色谱－串联质谱法测定猪肉中5种α2受体激动剂残留量方法的研究

Determination of Five Alpha-agonists in Pork by Ultra Performance Liqμid Chromatography-Tandem Mass Spectrometry

关键词:  α2受体激动剂  猪肉  超高效液相色谱-串联质谱法

Key words:  Alpha-agonists  Pork  Ultra performance liquid chromatography-tandem mass spectrometry

摘要:

建立了检测猪肉中5种α2受体激动剂的超高效液相色谱-串联质谱(UPLC/MS/MS)分析方法。样品加入碱性缓冲液,在再经过乙酸乙酯提取,浓缩、净化后用乙腈-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等5种Alpha受体激动剂标准曲线在0.5～100 ng/mL浓度范围内线性良好。线性相关系数(r)均大于0.99；在1~50 ng/g添加水平下,5种Alpha受体激动剂加标回收率在60～80%,相对标准偏差(RSD)均小于10%(n=6)；本方法对猪肉中5种Alpha受体激动剂的定量限为5 ng/g (S/N＞10),检出限为1 ng/g (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 five Alpha-agonists in pork. Five Alpha-agonists extracted by buffer(pH=11.3)from pork, 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?. Five Alpha-agonists were detected in positive ion mode using multiple reactions monitoring (MRM). The quantitative analysis was finished in 10.0 min. Results showed that in the range of 0.5 to 100 ng/Ml, the standard curves for five alpha-agonists were in good linearity , the correlation coefficients ( r) were greater than 0. 99. The recoveries for five alpha-agonists at the addition of four levels (1~50 ng/g) were 60% to 80% and the relative standard deviation (RSD) for the determination of five alpha-agonists 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 five alpha-agonists were found to be 5 ng/g and 1 ng/g, respectively.