高效液相色谱−串联质谱法测定猪组织中泰地罗新残留

    Determination of tildipirosin residues in swine tissues by high performance liquid chromatography-tandem mass spectrometry

    • 摘要:
      目的  建立适用于猪组织中泰地罗新残留检测的高效液相色谱−串联质谱法。
      方法  猪组织(肌肉、肝脏、肾脏和皮脂)样品经0.1 mol·L–1磷酸二氢钾溶液提取,上清液采用HLB固相萃取柱浓缩净化,Phenomenex Luna Omega C18色谱柱梯度洗脱,采用电喷雾正离子扫描和多反应监测(MRM)模式对泰地罗新进行分析,采用基质匹配法对泰地罗新含量进行标准校正。
      结果  泰地罗新添加剂量在肌肉中25~2 400 ng·g–1、肝脏中25~2 500 ng·g–1、肾脏中25~2 000 ng·g–1和皮脂中25~1 600 ng·g–1的范围内,与特征离子峰面积呈良好的线性关系(r2 ≥ 0.99)。猪组织添加泰地罗新样品中肌肉、肝脏、肾脏和皮脂的检测限均为10 ng·g–1,定量限均为25 ng·g–1。对猪组织在定量限、1/2MRL、MRL、2MRL这4个剂量下进行泰地罗新的添加回收试验,各组织中的批内平均回收率为85.6%~105.0%,批内回收率相对标准偏差2.3%~9.5%,批间回收率相对标准偏差4.7%~7.6%。
      结论  该方法简单易行,灵敏度高且特异性强,可用于猪组织中泰地罗新残留量的分析测定。

       

      Abstract:
      Objective  To establish a reliable HPLC-MS/MS (High performance liquid chromatography-tandem mass spectrometry) method suitable for determing tildipirosin residues in swine tissues.
      Method  Swine tissue samples, including muscle, liver, kidney and skin-fat were extracted with 0.1 mol·L–1 KH2PO4 buffer solution. The supernatant fluids were enriched and purified using HLB solid-phase extraction column, and gradiently eluted by Phenomenex Luna Omega C18 liquid chromatography column. The analytes were then detected using triple-quadrupole mass spectrometry in positive electrospray ionization and multiple reaction monitoring (MRM) mode. The matrix-matched method was used to calibrate tildipirosin content.
      Result  Tildipirosin contents presented good linear relationships (r2>0.99) with characteristicion peak area in the ranges of 25–2 400 ng·g–1 in muscle, 25–2 500 ng·g–1 in liver, 25–2 000 ng·g–1 in kidney and 25–1 600 ng·g–1 in skin-fat. All the limits of detection and quantitation in muscle, liver, kidney and skin-fat samples added tildipirosin were 10 and 25 ng·g–1, respectively. The recovery experiments of tildipirosin in swine tissues were setted in four dosage levels, including limit of quantitation, 1/2 maximum residue limit (MRL), MRL and 2MRL, and the mean intra-batch recoveries of tildipirosin in all analytes ranged from 85.6% to 105.0%. The relative standard deviations of intra-batch and inter-batch recoveries were in the ranges of 2.3%–9.5% and 4.7%–7.6%, respectively.
      Conclusion  The established method is simple, practicable, and with high sensitivity and specificity. It can be applied to determine tildipirosin residues in swine tissues.

       

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