QuEChERS-高效液相色谱-串联质谱法同时测定猪肉中氯霉素、氟苯尼考和五氯酚的残留量

Simultaneous determination of chloramphenicol, florfenicol and pentachlorophenol in pork by QuEChERS-high performance liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  高效液相色谱-串联质谱法  氯霉素  氟苯尼考  五氯酚

英文关键词:QuEChERS  high performance liquid chromatography-tandem mass spectrometry  chloramphenicol  florfenicol  pentachlorophenol

中文摘要:

      目的 建立QuEChERS-高效液相色谱-串联质谱法快速测定猪肉中氯霉素、氟苯尼考和五氯酚的分析方法。方法 以乙腈为提取溶剂, 加入正己烷除脂, 氮吹浓缩乙腈定容后经C18填料萃取净化, 在高效液相色谱-串联质谱仪上采用电喷雾负离子扫描模式(electron spray ionization, ESI-)测定, 内标法定量。结果 该方法在1.0~50.0 μg/L范围内有良好的线性关系, 相关系数均大于0.99, 氯霉素和氟苯尼考的方法检出限为0.1 μg/kg, 五氯酚的方法检出限为0.06 μg/kg。平均回收率在81.1%～115.8%范围, 相对标准偏差在4.2%~11.8%范围。结论 本方法操作简便, 准确度和精密度好, 可同时检测猪肉中氯霉素、氟苯尼考和五氯酚的残留量。

英文摘要:

      Objective To establish a rapid method for the determination of chloramphenicol, florfenicol and pentachlorophenol in pork by QuEChERS-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The analyte was extracted with acetonitrile. N-hexane was used to remove the fat. C18 purification material was applied to purify the concentrated sample. The analyte was determined by electrospray negative ion scanning mode (electron spray ionization) with HPLC-MS/MS, and quantified by the internal standard method. Results The method showed good linear relationship in the range of 1.0–50.0 μg/L for analyte, and the correlation coefficient square was greater than 0.99. The limits of detection (LOD) of chloramphenicol and florfenicol were 0.1 μg/kg, and pentachlorophenol was 0.06 μg/kg. The average recoveries were 81.1%–115.8%, and the relative standard deviation (RSD) was 4.2%–11.8%. Conclusion This method is easy to operate, accurate and precise. Chloramphenicol, florfenicol and pentachlorophenol in pork can be detected simultaneously.