液相色谱-串联质谱法检测蜂蜜中氨苯砜及其代谢产物残留量

Determination of dapsone and its metabolite residues in honey by liquid chromatography-tandem mass spectrometry

中文关键词:  氨苯砜  N-乙酰氨苯砜  液相色谱串联质谱法  蜂蜜  残留量

英文关键词:dapsone  mono-N-acetyldapsone  liquid chromatography-tandem mass spectrometry  honey  residues

中文摘要:

      目的 建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, UPLC–MS/MS)检测蜂蜜中氨苯砜及其代谢产物N-乙酰氨苯砜的分析。方法 样品经磷酸盐缓冲液(pH=9)提取, 经Oasis HLB固相萃取小柱净化, 富集后采用液相色谱-电喷雾质谱进行检测, 以正离子多反应监测模式测定, 同位素内标法定量。结果 氨苯砜及其代谢物产物的线性范围为0.5~50 ng/mL, 加标回收率为90.0%~110.0%, 相对标准偏差小于10.0%(n=6); 方法检出限为0.1 μg/kg, 定量限为0.5 μg/kg。结论 该方法快速、准确、灵敏, 适合用于蜂蜜中氨苯砜及其代谢物N-乙酰氨苯砜残留的确证检测。

英文摘要:

      Objective To establish a method for deternimation of dapsone and its metabolite residues in honey using liquid chromatography-tandem mass spectrometry (LC–MS/MS). Methods The samples were extracted by phosphate buffer solution (pH=9) and purified by Oasis HLB solid phase extraction (SPE). After enriched, the samples were detected by liquid chromatography-electrospray mass spectrometry (LC-MS/MS) with positive electrospray ionization (ESI+) mode and multiple reactions monitoring (MRM), and internal standard method was used for quantitative determination. Results Dapsone and its metabolit had good linear relationships in the range of 0.5- 50 ng/mL. The average recoveries of dapsone and its metabolite from spiked sample at 3 concentration levels were between 90% and 110% and the relative standard deviations (RSDs) were less than 10% (n=6). The limits of detection were 0.1 μg/kg and the limits of quantitation were 0.5 μg/kg. Conclusion This method is rapid, accurate and sensitive, which is suitable for detecting dapsone and its metabolite in honey samples.