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  

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

作　　者：刘正才[1] 张琼[1] 杨方[1] 林永辉[1] 刘素珍[1] 苏芝娇[1] 

机构地区：[1]福建出入境检验检疫局福建省检验检疫技术研究重点实验室,福建福州350001

出　　处：《食品科学》2015年第4期198-201,共4页Food Science

基　　金：公益性行业(质检)科研专项(201310143-02);福建省科技项目(2012Y6001)

摘　　要：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。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.

关 键 词：亲水作用色谱-电喷雾串联质谱法 水产品 氟苯尼考胺 残留检测 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]