摘要
建立了动物源性食品中特布他林、西马特罗、沙丁胺醇、非诺特罗、氯丙那林、莱克多巴胺、克仑特罗、妥布特罗和喷布特罗等9种β-受体激动剂残留检测的超高效液相色谱-串联质谱方法。样品经酶解后,用高氯酸去除蛋白质等杂质,调节上清液的pH值后,分别用乙酸乙酯和叔丁基甲醚进行萃取,再用MCX固相萃取柱净化,然后用WatersAcquityUPLCBEHC18色谱柱(50mm×2.1mm,1.7μm)分离,以0.1%甲酸乙腈溶液和0.1%甲酸水溶液为流动相进行梯度洗脱,外标法定量。结果表明:9种β-受体激动剂在0.25～5μg/kg的空白添加浓度范围内呈良好的线性关系,相关系数(r)均大于0.990;特布他林等8种药物的检出限为0.1μg/kg,定量限为0.25μg/kg;喷布特罗的检出限为0.25μg/kg,定量限为0.5μg/kg。从0.5,1和2μg/kg共3个添加浓度的检测结果可以看出,9种药物的平均回收率为87.1%～108.6%,批内、批间相对标准偏差(RSD)均小于20%。该方法具有简便快捷、灵敏度高、定性准确等特点。
An ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）method was established for the simultaneous determination of terbutaline,cimaterol,salbutamol,fenoterol,clorprenaline,ractopamine,clenbuterol,tulobuterol,penbutolol residues in animal derived foods.After enzymolysis,the samples were extracted by perchloric acid,centrifuged,neutralized,followed by liquid-liquid extraction with ethyl acetate and tert-butyl methyl ether,separately.The combined extracts were applied to a solid phase extraction MCX cartridge for cleanup.The separation of β-agonists was performed on Waters Acquity UPLC system with a BEH C18 column（50 mm×2.1 mm,1.7 μm）and the gradient elution solvent of acetonitrile（containing 0.1% formic acid）and water（containing 0.1% formic acid）at a flow rate of 0.3 mL/min.The method was quantified by external standard method.The calibration curves were good linear between the peak areas and the concentrations of 0.25-5 μg/kg with the correlation coefficient r〉0.990.The limit of detection of the 8 β-agonists was 0.1 μg/kg,and the limit of quantification was 0.25 μg/kg.The limit of detection of penbutolol was 0.25 μg/kg,and the limit of quantification was 0.5 μg/kg.The average recoveries from spiked animal tissues at three concentrations of 0.5,1 and 2 μg/kg ranged 87.1%-108.6%.The relative standard deviations of intra-and inter-batch were both less than 20%.
出处
《色谱》
CAS
CSCD
北大核心
2008年第6期709-713,共5页
Chinese Journal of Chromatography
基金
国家科技支撑计划课题项目(No.2006BAD31B09)
关键词
超高效液相色谱-串联质谱
β-受体激动剂
残留
动物源性食品
ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）
β-agonists
residue
animal derived food
作者简介
通讯联系人：孙雷，硕士，助理研究员，主要从事兽药残留方面的工作．Tel：（010）62103654，E-mail：sunlei@ivdc．gov．cn．
