- Chinese Core Journal
- Chinese Science Citation Database (CSCD) Source journal
- Journal of Citation Report of Chinese S&T Journals (Core Edition)
| 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
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To establish a reliable HPLC-MS/MS (High performance liquid chromatography-tandem mass spectrometry) method suitable for determing tildipirosin residues in swine tissues.
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.
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.
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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