UPLC-MS/MS测定水产品中氟喹诺酮类药物前处理优化

Optimization of sample preparation for the determination of fluoroquinolone antibiotics residues in aquatic products by UPLC - MS /MS

建立了一种快速、灵敏的超高效液相色谱串联质谱法（UPLC-MS/MS）同时定性和定量测定水产品中6种氟喹诺酮类（FQs）药物残留.考察了提取液类型、提取液甲酸体积分数、净化方式、脱水剂用量等影响浓缩富集效果的因素,确立了样品采用酸化乙腈溶液提取、正己烷脱脂并以无水硫酸钠除水等步骤.在电喷雾-多反应监测正离子模式下,色谱分离柱选用BEH C18色谱柱,流动相选用0.1%甲酸水溶液-乙腈梯度洗脱,流速为0.20 mL/min.结果表明,6种氟喹诺酮类标准品均在1~1 000μg/L内线性关系良好（R2均≥0.998）,在2~100μg/kg添加范围内平均回收率在76.9%~95.9%,相对标准偏差在4.8%~9.2%,最低检测限和定量限分别为0.1和0.2μg/kg.

The preparation was optimized for the quantitative and qualitative determination of six fluoroquinolone antibiotics（FQs） in muscles of aquatic products using ultra-performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry （ UPLC - MS/MS）. Types of extraction, content of formic acid in extraction solution, styles of the cleanup, and amount of dehydrates were discussed for the purpose of reaching the optimal result of sample preparation. Extraction of the FQs was carried out with acid acetonitrile and defatted with n-hexane, while the water in the muscle was removed by sodium sulfate. Separation of the FQs was achieved by using a BEH C18 column under gradient elution at flow rate of O. 20 mL/min with the mobile phases being composed of 0. 1% formic acid solution and acetonitrile. The mass spectrometer was operated in positive ion mode using electrospray ionization in the multiple reaction monitoring （MRM） mode. The standard curves were linear （R2 ≥ 0. 998 ） over the concentration ranging from 1.0 to 1 000 μg/L when the limit of detection （LOD） and limit of quantification （LOQ） were 0. 1 and 0. 2 μg/kg, respectively. Recoveries of the FQs in spiked samples（fish, shrimp and crab） arranging from 2 to 100μg/kg were between 76.9% and 95.9% with the relative standard deviation between 4. 8% and 9.2%.