色谱

色谱

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超高效液相色谱-串联质谱法检测动物源性食品中残留的9种β-受体激动剂

孙雷1,张骊1,朱永林2,王树槐1,汪霞1   

  1. 1.China Institute of Veterinary Drug Control, Beijing 100081, China; 2.Jiangsu Provincial Test Centre of Animal By-Product Quality, Nanjing 210036, China
  • 收稿日期:2008-05-26 修回日期:2008-08-26 出版日期:2008-11-30 发布日期:1983-06-25
  • 通讯作者: 孙雷
  • 基金资助:
    国家科技支撑计划课题项目(No. 2006BAD31B09)

Simultaneous determination of nine β-agonist residues in animal derived foods by ultra performance liquid chromatography-tandem mass spectrometry

SUN Lei1, ZHANG Li1, ZHU Yonglin2, WANG Shuhuai1, WANG Xia1   

  1. 1.China Institute of Veterinary Drug Control, Beijing 100081, China; 2.Jiangsu Provincial Test Centre of Animal By-Product Quality, Nanjing 210036, China
  • Received:2008-05-26 Revised:2008-08-26 Online:2008-11-30 Published:1983-06-25
  • Contact: SUN Lei

PDF

808

被引次数

124

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Waters Acquity UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7 μm)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0.25～5 μg/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0.1 μg/kg,定量限为0.25 μg/kg;喷布特罗的检出限为0.25 μg/kg,定量限为0.5 μg/kg。从0.5,1和2 μg/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。

关键词: β-受体激动剂, 残留, 超高效液相色谱-串联质谱, 动物源性食品

Abstract: 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%.

Key words: animal derived food , residue, β-agonists, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)