液相色谱串联质谱法测定猪肉中的安定残留

Determination of Diazepam with Liquid Chromatography-Tandem Mass Spectrometry in Swine Muscle

建立了猪肌肉中安定的高效液相色谱-串联质谱检测方法。用乙腈提取猪肌肉组织中的药物,经HLB固相柱净化,采用正电喷雾离子源,在多反应监测（MRM）模式下测定,三对定性离子对（m/z）分别为：285.4〉154.0、285.4〉193.0和285.4〉257.0,定量离子对m/z为285.4〉154.0。结果表明：安定在0.1～100 ng/mL内线性良好,相关系数r为0.998 5。在0.5、2、10μg/kg添加水平下,加标回收率为68.2%～97.6%,变异系数（CV）在2.2%～7.8%之间,检测限为0.1μg/kg,定量限为0.5μg/kg。

A method for determination of diazepam in swine muscle with liquid chromatography - tandem mass spectrometry was established. The drug in swine muscle was extracted with aeetonitrile, purified by HLB SPE columns, and detected by positive electrospray ionization. Multiple reaction monitoring （MRM） of three parent - daughter ion pairs ： （m/z） 285.4 〉 154.0, 285.4 〉 193.0 and 285.4 〉 257.0. The ion pair of 285.4 〉 154.0 was used for quantitation. Results showed that in the range of 0.1 - 100 ng/mL the standard curves for diazepam were in good linearity, the coefficient of correlation （r） was 0.998 5. The recoveries for diazepam at the addition of three levels （0.5, 2, 10 μg,/kg） were ranged from 68.2% - 97.6% with the coefficients of variation from 2.2% - 7.8%. The limit of detection and limit of quantity was 0.1 μg/kg and 0.5 μg/kg respectively.