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    王文湘, 闫超群, 华成云, 等. 高效液相色谱−串联质谱法测定猪组织中泰地罗新残留[J]. 华南农业大学学报, 2018, 39(6): 32-38. doi: 10.7671/j.issn.1001-411X.2018.06.006
    引用本文: 王文湘, 闫超群, 华成云, 等. 高效液相色谱−串联质谱法测定猪组织中泰地罗新残留[J]. 华南农业大学学报, 2018, 39(6): 32-38. doi: 10.7671/j.issn.1001-411X.2018.06.006
    shu
    WANG Wenxiang, YAN Chaoqun, HUA Chengyun, LI Guoji, WANG Bo, GU Xin, CAO Ying, HUANG Shixin, HUANG Xianhui. Determination of tildipirosin residues in swine tissues by high performance liquid chromatography-tandem mass spectrometry[J]. Journal of South China Agricultural University, 2018, 39(6): 32-38. DOI: 10.7671/j.issn.1001-411X.2018.06.006
    Citation: WANG Wenxiang, YAN Chaoqun, HUA Chengyun, LI Guoji, WANG Bo, GU Xin, CAO Ying, HUANG Shixin, HUANG Xianhui. Determination of tildipirosin residues in swine tissues by high performance liquid chromatography-tandem mass spectrometry[J]. Journal of South China Agricultural University, 2018, 39(6): 32-38. DOI: 10.7671/j.issn.1001-411X.2018.06.006
    shu

    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
    • 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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