高效液相色谱-串联质谱法快速测定鱼肉中4种氟喹诺酮类药物残留  

A Rapid High-performance Liquid Chromatography-Tandem Mass Spectrometric Method for Determination of 4 Fluoroquinolones Residues in Fish Meat

作　　者：黄优生[1] 刘波平[1] 朱筱玲[1] 李桂生[1] 

机构地区：[1]江西省分析测试中心,江西南昌330029

出　　处：《食品科学》2010年第2期127-130,共4页Food Science

摘　　要：建立快速测定鱼肉中4种氟喹诺酮类药物残留的高效液相色谱-串联质谱方法。采用酸性乙腈提取样品中的氟喹诺酮药物残留,然后用正己烷脱脂,氮吹浓缩定容后,用反相液相色谱分离,以液相色谱-串联质谱仪测定,外标法定量。该法对4种氟喹诺酮类药物的线性范围为2～40μg/kg,相关系数(r2)大于0.997,在4、10、20μg/kg3个添加水平范围内的回收率为79.9%～98.1%,相对标准偏差为2.7%～8.7%,检出限为0.1～0.4μg/kg,定量限为0.3～1.0μg/kg。结果表明,该方法简便快速、灵敏度高、重现性好、选择性强,适用于鱼肉中氟喹诺酮类药物残留的定量测定。A high-performance liquid chromatography-tandem mass spectrometric （HPLC-MS/MS） method was developed for the simultaneous determination of 4 fluoroquinolone antibiotic residues in fish meat. In the method, analytes were extracted with acidified acetonitrile, cleaned up with n-hexane, concentrated to dryness under nitrogen, redissolved in 1 mL of mixed solution of acetonitrile and 1% formic acid （1：9, V/V）, separated on a RP-HPLC column, detected by HPLC-MS/MS with positive electrospray ionization （ESP） in multiple reaction monitoring （MRM） mode, and quantified using an external standard method. The standard curves for all analytes exhibited good linearity over the concentration range of 2 - 40 μ g/kg with correlation coefficients （r2） beyond 0.997. The recoveries of 4 fluoroquinolone antibiotics in fish meat samples spiked at concentration levels of 4, 10 lag/kg and 20 μg/kg ranged from 79.9% to 98.1%, with relative standard deviations between 2.7 % and 8.7 %. The limits of detection （LOD） and limits of quantification （LOQ） of the developed method were in the ranges of 0.1 -- 0.4 μg/kg and 0.3 -- 1.01μg/kg, respectively. This method is characterized by simplicity, rapidity, high sensitivity, good reproducibility and better selectivity, and therefore can be used for identification and determination of fluoroquinolones in fish meat.

关 键 词：高效液相色谱-串联质谱(HPLC-MS/MS)法 氟喹诺酮 残留 鱼肉 

分 类 号：TS207.3[轻工技术与工程—食品科学] O657.63[轻工技术与工程—食品科学与工程]