液相色谱-串联质谱法检测调味品中碱性橙2的残留量

Determination of basic orange Ⅱ residues in condiment by liquid chromatography-tandem mass spectrometry

中文关键词:  碱性橙2  液相色谱串联质谱法  固相萃取  调味品  残留量

英文关键词:basic orange Ⅱ  liquid chromatography-tandem mass spectrometry  solid phase extraction  condiment  residues

中文摘要:

      目的 建立液相色谱-电喷雾质谱法(liquid chromatography-tandem mass spectrometry, UPLC–MS/MS) 检测调味品中碱性橙2的分析方法。方法 样品经酸化乙腈提取, 正己烷去脂后, 经固相萃取小柱净化, 氮气吹干进行富集后, 用乙腈溶解, 再采用液相色谱-电喷雾质谱进行检测, 以正离子多反应监测模式测定, 外标法定量。结果 碱性橙2的线性范围为0.2~20 ng/mL, 线性方程为Y=0.0993X?0.0106 (r=0.9999), 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1 μg/kg, 定量限为3 μg/kg。结论 该方法 快速、准确、灵敏, 适合用于食品中碱性橙2的确证检测。

英文摘要:

      Objective To establish a method for the deternamiton of basic orange Ⅱ residues in condiment by liquid chromatography-tandem mass spectrometry. Methods The sample was extracted by acidizing acetonitrile, deacidized by n-hexane, and purified by solid-phase extraction and enriched by nitrogen blow-dry. Then it was dissolved by acetonitrile and detected by liquid chromatography-mass spectrometry (electronic spray ion) with the cationic multiple reaction monitoring model, and quantified by external standard method. Results Basic orange Ⅱ had good linear relationships in the range of 0.2-20 ng/mL, and the linear equation was Y=0.0993X-0.0106 (r=0.9999). The average recoveries at 3 concentration levels were between 90% and 110%, and the relative standard deviations (RSDs) were less than 10.0% (n=6). The limits of detection (LODs) were 1 μg/kg and the limits of quantitation were 3 μg/kg. Conclusion This method is rapid, accurate and sensitive, which is suitable for detecting basic orange Ⅱ in condiment samples.