超高效液相色谱-串联质谱法测定兔肉中加米霉素残留量

Determination of gamithromycin residues in Oryctolagus cuniculus meat by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  兔肉  加米霉素  残留量

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  Oryctolagus cuniculus meat  gamithromycin  residues

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测兔肉中加米霉素残留量的方法。方法 兔肉样品采用乙腈提取, 经正己烷脱脂后, 通过Qasis MCX固相萃取柱完成净化处理, 采用 Xevo TQ-XS UPLC-MS/MS仪, 经梯度洗脱, 电喷雾离子源正离子扫描模式(electrospray ionization positive, ESI+), 多反应监测(multiple reaction monitoring, MRM), 内标法定量进行分析。结果 加米霉素进样质量浓度在0.25~50.00 ng/mL范围内与目标物峰面积具备优异线性相关性(r2>0.999); 检出限为0.25 μg/kg, 定量限为0.50 μg/kg; 于0.5、1.0、50.0 μg/kg 3个加标水平下, 平均回收率介于76.8%~102.3%, 批内及批间相对标准偏差均低于15% (n=6)。结论 本方法灵敏、准确, 适用于兔肉中加米霉素残留量检测。本研究可为兔肉产品兽药残留监测与质量安全控制提供科学依据与技术支持。

英文摘要:

      Objective To establish a method for the detection of gamithromycin residues in Oryctolagus cuniculus meat by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Oryctolagus cuniculus meat samples were extracted using acetonitrile, subjected to defatting with n-hexane, and further purified with Qasis MCX solid-phase extraction cartridges, and analyzed by Xevo TQ-XS UPLC-MS/MS with gradient elution, electrospray ionization positive scan mode (ESI+), multiple reaction monitoring (MRM) and internal standard method were applied for quantitative analysis. Results There was an excellent linear correlation between the target peak area and the injection mass concentrations of gamithromycin at the range of 0.25–50.00 ng/mL (r2>0.999). The limit of detection and limit of quantitation were 0.25 μg/kg and 0.50 μg/kg. The average recoveries ranged from 76.8% to 102.3%, with intra-batch and inter-batch relative standard deviations both lower than 15% (n=6) at the addition levels of 0.5, 1.0 and 50.0 μg/kg. Conclusion The method is sensitive, accurate, and suitable for the detection of residues of gamithromycin in Oryctolagus cuniculus meat. This study can provide scientific basis and technical support for the monitoring and quality safety control of veterinary drug residues in Oryctolagus cuniculus meat products.