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超高效液相色谱-串联质谱法同时测定动物源性食品中9种β-激动剂残留量

[Simultaneous determination of nine beta-agonist residues in animal derived foods by ultra performance liquid chromatography-tandem mass spectrometry].

作者信息

Sun Lei, Zhang Li, Zhu Yonglin, Wang Shuhuai, Wang Xia

机构信息

China Institute of Veterinary Drug Control, Beijing 100081, China.

出版信息

Se Pu. 2008 Nov;26(6):709-13.

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 beta-agonists was performed on Waters Acquity UPLC system with a BEH C18 column (50 mm x 2.1 mm, 1.7 microm) 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 microg/kg with the correlation coefficient r > 0.990. The limit of detection of the 8 beta-agonists was 0.1 microg/kg, and the limit of quantification was 0.25 microg/kg. The limit of detection of penbutolol was 0.25 microg/kg, and the limit of quantification was 0.5 microg/kg. The average recoveries from spiked animal tissues at three concentrations of 0.5, 1 and 2 microg/kg ranged 87.1% - 108.6%. The relative standard deviations of intra- and inter-batch were both less than 20%.

摘要

建立了一种超高效液相色谱-串联质谱(UPLC-MS/MS)法,用于同时测定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、克伦特罗、妥布特罗、喷布洛尔的残留量。样品经酶解后,用高氯酸提取,离心,中和,再分别用乙酸乙酯和叔丁基甲基醚进行液-液萃取。合并萃取液,通过固相萃取MCX柱进行净化。在Waters Acquity UPLC系统上,使用BEH C18柱(50 mm×2.1 mm,1.7 µm),以乙腈(含0.1%甲酸)和水(含0.1%甲酸)为梯度洗脱溶剂,流速为0.3 mL/min,对β-激动剂进行分离。该方法采用外标法定量。峰面积与浓度在0.25 - 5 μg/kg之间校准曲线线性良好,相关系数r>0.990。8种β-激动剂的检出限为μg/kg,定量限为0.25 μg/kg。喷布洛尔的检出限为0.25 μg/kg,定量限为0.5 μg/kg。在0.5、1和2 μg/kg三个浓度水平下,动物组织加标回收率为87.1% - 108.6%。批内和批间相对标准偏差均小于20%。

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