超高效液相色谱-串联质谱法测定饲料中苯乙醇胺A的残留量

建立了超高效液相色谱-串联四极杆质谱测定饲料中苯乙醇胺A残留的分析方法。用磷酸甲醇溶液提取饲料中的苯乙醇胺A,经MCX柱净化、富集后,在正离子模式下以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱,Waters超高效BEH C18色谱柱(100 mm×2.1 mm, 1.7 μm)分离,电喷雾离子源电离,多反应监测(MRM)模式下进行定量和定性分析。结果表明,苯乙醇胺A在0.5～100 μg/kg范围内的峰面积与含量线性相关(相关系数(r)﹥0.999),其定量限(S/N)为10 μg/kg,方法回收率为79.6%～86.2%,相对标准偏差(RSD)为3.1%～6.7%。多次测定饲料样品表明该方法操作方便、测定结果可靠。

Determination of phenylethanolamine A residue in feeds by ultra performance liquid chromatographytandem mass spectrometry

A method was developed for the determination of the residue of phenylethanolamine A in feeds by ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS). The phenylethanolamine A in sample was extracted with phosphoric acid methanol solution. The extract was purified and concentrated by an MCX column. In the positive mode, an ultra-performance BEH C18 column (100 mm×2.1 mm, 1.7 μm) was used to separate the phenylethanolamine A, and the separation was carried out on a Waters UPLC system by using gradient elution with acetonitrile and 0.1%(v/v)formic acid aqueous solution as the mobile phases at a flow rate of 0.4 mL/min. The qualitative and quantitative analysis was carried out by multi-reaction monitoring (MRM) mode, in which the analyte was ionized by electrospray ionization interface (ESI). The results showed that, the calibration curve was linear in the range of 0.5~100 μg/kg (r﹥0.999), the limit of quantification (S/N ＞ 10) was 10 μg/kg, the recoveries ranged from 79.6% to 86.2%, and the relative standard deviations (RSDs) were between 3.1% and 6.7%. The real sample tests showed that the method is convenient and reliable.