亲水作用色谱-电喷雾串联质谱法测定水产品中的氟苯尼考胺的残留量

建立亲水作用色谱-电喷雾串联质谱测定水产品中氟苯尼考胺残留量的测定方法。样品用碱性乙酸乙酯提取,以正己烷和脂肪吸附材料去除油脂,用5 mmol/L乙酸铵溶液(含0.2%甲酸)和乙腈作为流动相,以梯度洗脱方式在Acquity UPLC BEH HILIC柱(55 mm×2.1 mm,1.7μm)色谱柱上分离,以电喷雾离子源正离子模式进行质谱分析,基质外标法定量。结果表明,氟苯尼考胺的质量浓度在0.1~20μg/L范围内呈良好的线性,相关系数(r2)大于0.990。在1.0~50.0μg/kg加标水平下,虾、黄鱼、鳗鱼、烤鳗的平均回收率为70.5%~87.7%,相对标准偏差为4.8%~11.6%,定量限为1.0μg/kg。该方法简单、灵敏、稳定,可满足水产品中氟苯尼考胺残留量的检测和确证需要。

Determination of Florfenicol Amine in Aquatic Products by Hydrophilic Interaction Chromatography-Tandem Mass Spectrometry

A method for the determination of florfenicol amine (FFA) in aquatic products was developed by hydrophilic
interaction chromatography-tandem mass spectrometry (HILIC-MS-MS). Samples were extracted with alkalinified ethyl
acetate and cleaned up with n-hexane and lipid adsorbent (LAS). An Acquity UPLC BEH HILIC (55 mm × 2.1 mm, i.d.
1.7 μm) colunm was used for the separation by gradient elution program using acetonitrile-5 mmol/L ammonium acetate
containing formic acid (0.2%) as the mobile phase, and an electrospray ion trap mass spectrometer was used in the positive
ion mode. The FFA was quantified by the matrix-matched external standard method. The results showed that the established
method had a good linear correlation (r2 > 0.990) in the range of 0.1–20 μg/L. The average recoveries of FFA at spiked level
of 1.0–50.0 μg/kg were in the range of 70.5%–87.7% with relative standard deviations (RSDs) of 4.8%–11.6%. The limit of
quantization (LOQ) was 1.0 μg/kg. This method proved to be simple, sensitive, accurate, and suitable for the determination
and confirmation of FFA in aquatic products.