高效液相色谱-串联质谱法测定蜂蜡中痕量氯霉素残留

Determination of trace chloramphenicol residue in beeswax by high performance liquid chromatography tandem mass spectrometry

中文关键词:  固相萃取净化  高效液相色谱-串联质谱法  蜂蜡  氯霉素

英文关键词:solid phase extraction  high performance liquid chromatography-tandem mass spectrometry method  beeswax  chloramphenicol

中文摘要:

      目的 建立正己烷预处理-固相萃取净化-高效液相色谱-串联质谱法检测蜂蜡中痕量氯霉素的分析方法。方法 试样采用正己烷预溶解, 经水提取后进行亲水亲脂平衡(hydrophilic-lipophilic-balance, HLB)固相萃取小柱净化, 用Accucore XL C18柱分离, 多反应监测(multiple reaction monitoring, MRM)模式串联质谱进行测定, 内标法定量。结果 氯霉素在0.3~10 ng/mL范围内与峰面积具有较好的线性关系, 相关系数大于0.998。该方法检出限(S/N>3)为0.05 μg/kg, 方法定量限(S/N>10)为0.3 μg/kg, 在0.3、1.0和2.0 μg/kg 3个添加水平下的回收率为80.2%~105.2%, 相对标准偏差均小于8%(n=6)。结论 本方法快速、灵敏、准确, 适用于日常大批量蜂蜡样品中痕量氯霉素残留量的分析。

英文摘要:

      Objective To establish a method for the determination of trace chloramphenicol residue in beeswax by n-hexane pretreatment-solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry (SPE-HPLC-MS/MS). Methods The samples were predissolved with n-hexane and then extracted with water, purified by hydrophilic-lipophilic-balance(HLB)solid phase extraction cartridge, separated with Accucore XL C18 column, detected by multiple reaction monitoring (MRM) mode tandem mass spectrometry, and quantified by internal standard method. Results Chloramphenicol had a good linear relationship with peak area in the range of 0.3~10 ng/mL, and the correlation coefficient was greater than 0.998. The limits of detection (S/N>3) for chloramphenicol was 0.05 μg/kg, and the limits of quantification (S/N>10) was 0.3 μg/kg. The recoveries at the three addition levels of 0.3, 1.0 and 2.0 μg/kg were 80.2%~105.2%, and the relative standard deviations were all less than 8% (n=6). Conclusion This method is rapid, sensitive and accurate. It is suitable for the determination of chloramphenicol residue in large quantities of beeswax samples.