高效液相色谱-串联质谱法测定水产品中的喹乙醇

Determination of Olaquindox Residues in Aquatic Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

为测定水产品中喹乙醇的残留量，建立了高效液相色谱－串联质谱联用（HPLC—MS／MS）的测定方法。均质后的试样经水提取、液－液分配净化后。采用ZORBAXSB—C18色谱柱，并以0．1％乙酸＋乙腈（70＋30，体积分数）为流动相，色谱分离后直接进入串联质谱检测器。采用电喷雾正离子，多反应监测（MRM）模式检测，外标法定量。方法的检出限为10μg／kg，浓度在0．5—500μg／L范围内，线性良好（r=0．9989）。添加浓度在10—500μg／kg时，不同水产品基质的回收率在74．3％-93．5％之间。相对标准偏差（RSD）小于5．6％。本方法检出限低，回收率高，定性可靠．定量准确．适合于水产品中喹乙醇残留的检测．

A high performance liquid chromatography-tandem mass spectrometric （LC-MS/MS） method was developed for determination of olaquindox residues in aquatic products. The targeted analyte was extracted from homogenized samples with water, and purified with liquid-liquid extraction. Chromatographic separation was achieved by using ZORBAX SB-C18 column with an isocratic mobile phase consisting of 0.1% acetic acid and acetonitrile （70 ＋ 30, V/V ）. Analytical identification and quantification were performed using multiple reaction monitoring （MRM） with one precursor ion and three product ions as identifiers and electrospray ionization in positive mode. The detection limit of this method was 10 μg/kg . It was linearly ranged from 0.5 to 500 μg/L with the correlation coefficient 0.998 9. The recoveries for different matrices were 74.3% - 93.5% when the concentration of olaquindox ranged from 10 to 500μg/kg, the RSD was lower than 5.6%.