分散固相萃取/高效液相色谱-串联质谱法快速测定饲料中87种药物残留  

Dispersive Solid-phase Extraction Followed by Liquid Chromatography-Tandem Mass Spectrometry for Rapid Determination of 87 Kinds of Drug Residues in Feedingstuffs

作　　者：罗辉泰[1,2] 黄晓兰[1] 吴惠勤[1] 钟巧莉[1] 朱志鑫[1] 黄芳 林晓珊[1] 谢梦婷[1] 欧阳钢锋[2] 

机构地区：[1]中国广州分析测试中心广东省化学危害应急检测技术重点实验室,广东广州510070 [2]中山大学化学与化学工程学院,广东广州510275

出　　处：《分析测试学报》2015年第9期979-985,共7页Journal of Instrumental Analysis

基　　金：广州市科技计划项目(11BppZXcc6100034)

摘　　要：建立了分散固相萃取/高效液相色谱-串联质谱法（d SPE/LC-MS/MS）同时测定饲料中17种β-受体激动剂、18种β-内酰胺类、6种抗球虫类、5种大环内酯类、2种林可胺类、15种喹诺酮类、21种磺胺类及3种磺胺类增效剂等8类共计87种兽药的新方法。均质样品经0.1 mol/L Na2EDTA溶液分散后,以甲醇-乙腈（50∶50）超声提取,提取液用Bondesil-PSA吸附剂以分散固相萃取方式快速净化。待测物采用Poroshell EC-C18（100 mm×2.1 mm,2.4μm）色谱柱分离,在电喷雾离子源的正离子模式下以动态多反应监测（dynamic MRM）方式采集数据并作定性筛查和定量分析。87种药物在相应的浓度范围内线性良好,相关系数均大于0.99,在3个不同浓度加标水平下,平均回收率为63.7%~108.8%,相对标准偏差（RSD）为3.5%~15.2%,检出限（LOD,S/N≥3）和定量下限（LOQ,S/N≥10）分别为3~15μg/kg及10~50μg/kg。该方法灵敏、可靠,样品预处理简便、快速、价廉,适用于饲料中上述87种兽药的同时快速定性筛查和定量测定。A generic,rapid and simple multiresidue analytical method was developed and validated for determination of 8 classes of drugs including 17 β-agonists,18 β-lactams,6 coccidiostats,5 macrolides,2 lincosamides,15 quinolones,21 sulfonamides and 3 sulfonamides potentiators in feedingstuffs using dispersive solid- phase extraction（ d SPE） method and high performance liquid chromatography- tandem mass spectrometry（ HPLC- MS/MS）. The homogenized sample was dispersed by0. 1 mol/L Na2 EDTA solution,the analytes were extracted with a mixture of methanol- acetonitrile（ 50 ∶ 50） by ultrasonic,and then the extracts were purified by dispersive solid-phase extraction using Bondesil- PSA as adsorbent. Electrospray ionization mass spectrometry was operated in the positive mode using dynamic multiple reaction monitor（ d MRM） for the qualitative and quantitative analysis of 87 kinds of analytes after the separation on a Poroshell EC- C18（ 100 mm × 2. 1 mm,2. 4 μm）column. The correlation coefficients of linear calibration curves were over 0. 99 in the corresponding concentration range. The average recoveries of 87 drugs at three different spiked concentration levels ranged from 63. 7% to 108. 8%,with relative standard deviations（ RSDs） of 3. 5%- 15. 2%. The limits of detection（ LODs,S/N≥3） and quantitation（ LOQs,S/N≥10） were 3- 15 μg/kg and 10-50 μg/kg,respectively. The method was simple,rapid,sensitive and reliable,and was suitable for the determination of residues in feedingstuffs.

关 键 词：分散固相萃取 高效液相色谱-串联质谱法 动态多反应监测 饲料 β-受体激动剂 抗球虫类 抗生素 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]