超高效液相色谱-电喷雾串联质谱法对饲料中匹莫林的测定  

Determination of Pemoline in Feeds Using Ultra-performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry

作　　者：班付国[1] 方忠意[1] 刘素梅[1] 宋志超[1] 贾振民[1] 吴宁鹏[1] 

机构地区：[1]农业部畜禽产品质量安全检验测试中心(郑州),河南郑州450008

出　　处：《分析测试学报》2009年第6期705-708,共4页Journal of Instrumental Analysis

摘　　要：建立了超高效液相色谱-串联质谱测定饲料中匹莫林的方法。饲料样品经甲醇-乙腈溶液提取，取部分上清液氮气吹干，用甲醇和水分步溶解后用正己烷除脂，Waters Oasis HLB固相萃取小柱净化，然后用Waters Acquity UPLC BEH C18色潜柱（2．1mm×50mm．i.d．，1．7μm）分离，以甲醇和0．1％甲酸-水溶液为流动相进行梯度洗脱，外标法定量。对前处理及液相色谱和质谱条件进行优化。结果表明，匹莫林质量浓度在1～500μg／L范围内线性良好，相关系数大于0．999；在5．0～200μg/kg的添加水平下，匹莫林的平均加标回收率为77％～86％；相对标准偏差为4．4％～7．9％；方法的检出限低至2．0μg/kg，定量下限低至50μg／kg。该方法灵敏度高、稳定性好，可满足饲料中匹莫林残留的检测与确证的要求。An ultra-performance liquid chromatographic method with tandem mass spectrometric determination was developed for determination of pemoline in feeds. The sample was extracted by methanol - acetonitrile solution. The extract was evaporated to dryness under nitrogen, and redissolved by methanol and water, sequencely. The mixture was degreased by ethyl acetate and cleaned up on a Waters Oasis HLB solid phase extraction column. The separation of compounds was carried on a BEH C18 column （2. 1 mm× 50 mm i. d. , 1.7 μm） by a gradient elution using methanol（A） - water（ added 0. 1% formic acid） （B） as mobile phase with a flow rate of 0. 3 mL/min. The analyte was detected by tandem quadrupole mass spectrometry under multiple reaction monitoring （MRM） mode with positive electrospray ionization（ESI）. The method was quantified by external standard method. The experimental conditions were optimized. Under the optimal conditions, the calibration curve showed a good linearity over the concentration of pemoline in the range of 1 -500 μg/L with a correlation coefficient more than 0. 999. The detection limit （LOD） and the quantitative limit （LOQ） of pemoline were 2.0 μg/kg and 5.0 μg/kg, respectively. The average recoveries from spiked feeds samples at four concentration levels of 5.0, 10, 50 and 200 μg/kg ranged from 77% to 86% with relative standard deviations of 4.4% - 7.9% . The method showed a good repeatability and high sensitivity, and was suitable for the determination and confirmation of pemoline in feeds.

关 键 词：匹莫林 超高效液相色谱-串联质谱 饲料 

分 类 号：O657.63[理学—分析化学] TQ450.2[理学—化学]