快速检测动物源食品中63种激素残留
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摘要
建立了动物源食品中63种激素残留的快速检测方法。待测样品先经乙酸乙酯提取,再经氮气吹干乙腈定容,QuEChERS(45 mg PSA,25 mg C18,50 mg MgSO4)净化后以高效液相色谱-串联质谱检测。选择Agilent Poroshell 120 EC-C18色谱柱(2. 1 mm×150 mm,2. 7μm),梯度洗脱分离,电喷雾正离子模式下,采用预设定多反应监测(s MRM)模式扫描。实验结果表明,63种激素在相应的浓度范围内线性关系良好,相关系数均大于0. 995。不同空白肉类样品在3个加标水平实验下的回收率范围为61. 4%～119. 3%,63种激素的精密度(RSD,n=3)范围为0. 5%～16%,定量限(LOQ,S/N≥10)范围为0. 1～1μg/kg。该方法能够满足日常实际检测需求。
A multi-residue method was developed for the simultaneous determination of 63 hormones in foodstuff of animal origin( chicken,pork,and fish). Samples were extracted with ethyl acetate,dried by nitrogen,and dissolved with acetonitrile. Then purication was carried out by using a modied QuEChERS( 45 mg PSA,25 mg C18,50 mg MgSO4) method,and rapid analysis was carried out by high performance liquid chromatography-tandem mass spectrometry( HPLC-MS/MS). The hormones in the purified solution were separated on Agilent Poroshell 120 EC-C18( 2. 1 mm × 150 mm,2. 7μm) column and eluted by gradient elution. A scheduled multiple reaction monitoring( s MRM) in positive mode was adopted in mass spectrometry acquisition. As a result,the 63 hormones showed good linearity with all correlation coefficients( r) no less than 0. 9950 within the linear ranges. The mean recoveries at the three spiked levels were all in the range of 61. 4% ～ 119. 3%,and the relative standard deviations( RSDs) were between 0. 5% and 16%. The limits of quantification( LOQ,S/N≥10) for the 63 hormones were 0. 1 ～ 1μg/kg. The method can be applied for quantification of hormone residues in foodstuff of animal origin.
A multi-residue method was developed for the simultaneous determination of 63 hormones in foodstuff of animal origin( chicken,pork,and fish). Samples were extracted with ethyl acetate,dried by nitrogen,and dissolved with acetonitrile. Then purication was carried out by using a modied QuEChERS( 45 mg PSA,25 mg C18,50 mg MgSO4) method,and rapid analysis was carried out by high performance liquid chromatography-tandem mass spectrometry( HPLC-MS/MS). The hormones in the purified solution were separated on Agilent Poroshell 120 EC-C18( 2. 1 mm × 150 mm,2. 7μm) column and eluted by gradient elution. A scheduled multiple reaction monitoring( s MRM) in positive mode was adopted in mass spectrometry acquisition. As a result,the 63 hormones showed good linearity with all correlation coefficients( r) no less than 0. 9950 within the linear ranges. The mean recoveries at the three spiked levels were all in the range of 61. 4% ～ 119. 3%,and the relative standard deviations( RSDs) were between 0. 5% and 16%. The limits of quantification( LOQ,S/N≥10) for the 63 hormones were 0. 1 ～ 1μg/kg. The method can be applied for quantification of hormone residues in foodstuff of animal origin.
引文
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