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低延迟体积模式液相色谱-串联质谱法检测猪肉中盐酸克伦特罗残留量
Determination of Clenbuterol Residues in Pork by Liquid Chromatography-Tandem Mass Spectrometry with Low Delay Volume Mode
【摘要】 应用高效液相色谱-串联质谱法(HPLC-MS/MS),在液相部分采用低延迟体积模式,以盐酸克伦特罗-D9为内标,建立了快速测定猪肉中盐酸克伦特罗残留的检测方法。样品经过提取纯化后,采用C18色谱小柱进行梯度洗脱分离,电喷雾正离子MRM质谱检测。低延迟体积模式可实现洗脱液的快速梯度变换,仪器检测时间为2.0min;盐酸克伦特罗的保留时间为0.82min,其保留时间重现性好,所建立的标准曲线线性较好(R2=0.9993)。该方法的定量限(LOQ)为0.5μg/kg;当加标量为0.5、5、10μg/kg时,其回收率为81.2%~114.2%,相对标准偏差为6.4%~11.1%(n=6)。该方法检测速度快、灵敏度高、结果准确,可以满足实验室对猪肉中盐酸克伦特罗残留的高通量测试。
【Abstract】 A liquid chromatography-tandem mass spectrometry(LC-MS/MS) method for rapid determination of clenbuterol residues in pork by using clenbuterol-D9 as the internal standard was established.The pretreated samples were separated on a C18 column(50×2.1 mm,1.8 μm) and finally detected by positive electrospray ionization spectrometry(ESI+) with MRM mode.The detection time was 2.0 min and the retention time of clenbuterol was only 0.82 min.The limit of quantification of the method was 0.5 μg/kg.When spiked at 0.5 μg/kg,5 μg/kg and 10 μg/kg,the recoveries of clenbuterol ranged from 81.2% to 114.2%,with the relative standard deviations of 6.4%-11.1%(n=6).This method is characteristic of rapidity,high sensitivity and precision and can used for pork clenbuterol residues determination in high-throughput testing.
【Key words】 Clenbuterol; Low delay volume mode; Liquid chromatography-tandem mass spectrometry; Pork;
- 【文献出处】 分析科学学报 ,Journal of Analytical Science , 编辑部邮箱 ,2013年02期
- 【分类号】S859.84
- 【被引频次】1
- 【下载频次】109