高效液相色谱-电喷雾电离串联质谱法测定鸡肉、鸡蛋中氯霉素、甲砜霉素和氟苯尼考药物残留量

Determination of chlorampheincol, thiamphenicol and florfenicol residues in chicken and egg by high performance liquid chromatography- electrospray ionization-tandem mass spectrometry

中文关键词:  氯霉素  甲砜霉素  氟苯尼考  鸡肉  鸡蛋  高效液相色谱-电喷雾电离串联质谱法

英文关键词:chlorampheincol  thiamphenicol  florfenicol  chicken  egg  high performance liquid chromatography- electrospray ionization-tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-电喷雾电离串联质谱法测定鸡肉和鸡蛋中氯霉素、甲砜霉素、氟苯尼考残留量的分析方法。方法 准确称取5 g样品, 添加同位素内标氯霉素-d5后, 乙腈提取, LC-Si硅胶小柱净化, 正己烷进一步除脂, 0.22 μm滤膜过滤后高效液相色谱-电喷雾电离串联质谱测定。采用负离子电喷雾电离源, 多反应监测(multiple reaction monitoring, MRM)模式。结果 氯霉素、甲砜霉素和氟苯尼考在0.5~200 μg/L的系列浓度范围内线性良好, 其线性方程分别为Y=0.880X-0.215, Y=0.032X-0.076和Y=0.108X-0.115, 相关系数r2均大于0.990; 方法的检测限和定量限分别是0.05 μg/kg和0.1 μg/kg; 在加标水平在0.1~5.0 μg/kg的范围内, 鸡肉基质中平均回收率在87.01%~117.8%之间, 鸡蛋基质中平均回收率在80.74%~115.0%之间; 方法的日内精密度相对标准偏差在4.02%~9.88%之间, 日间精密度相对标准偏差在5.72%~12.78%之间。结论 该方法简单易行, 回收率好, 灵敏度高, 特异性好, 能满足目前大多数日常检测和监督的需要。

英文摘要:

      Objective To establish a method for the determination of chlorampheincols (CAP), thiamphenicol (TAP) and florfenicol (FF) residues in chicken and egg by high performance liquid chromatography-electrospray ionization- tandem mass spectrometry(HPLC-ESI-MS/MS). Methods The 5 g sample was taken and added an isotope standard (CAP-d5), then extracted with acetonitrile, cleaned up with LC-Si column, and degreased by hexane. The eluent was filtered through 0.22 um membrane and then analyzed by HPLC-ESI-MS/MS. Mass spectral acquisition was carried out by using electrospray ionization in negative ion mode with multiple reaction monitoring (MRM). Results The calibration curves of mixed standard solution showed good linearities in the concentrations from 0.5 to 200 μg/L with the correlation coefficients (r2) more than 0.990. The linear equations of CAP, TAP and FF were Y=0.880X-0.215, Y=0.032X-0.076 and Y=0.108X-0.115, respectively. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 0.05 μg/kg and 0.1 μg/kg, respectively. The average recoveries for the analysis of chicken samples spiked at the range of 0.1~5.0 μg/kg were in the range of 87.01%~117.8%, and egg samples were in the range 80.74%~115.0%. The relative standard deviations (RSDs) of within-day precision were 4.02%~9.88%, and intermediate precision were 5.72%~12.78%. Conclusion The proposed method is simple, accurate, and sensitive, which can meet the needs of daily detection and supervision.