固相分散净化-液相色谱质谱联用法检测辣椒粉中的碱性橙和碱性玫瑰精

Determination of Chrysoidine G and Rhodamine B in Paprika by Liquid Chromatography Tandem Mass Spectrometry with Solid Phase Dispersion Clean-upLiu Xiaochuang, LI Yonggang, LiuXiao,WEN Sheng

中文关键词:  液质联用仪  碱性橙  碱性玫瑰精  辣椒粉

英文关键词:HPLC-MS/MS  Chrysoidine G  Rhodamine B  Paprika

中文摘要:

      目的 建立辣椒粉中的碱性橙和碱性玫瑰精的高效液相色谱-串联四极杆质谱测定方法。方法 样品经乙腈超声提取后, 经ODS-C18和乙二胺-N-丙基硅烷(PSA)的固相分散净化后直接进样分析。使用安捷伦Zobax Eclipse Plus-C18(2.1 mm×100 mm, 1.8 μm)色谱柱分离, 以5 mmol/L乙酸铵-0.1%甲酸-乙腈为流动相, 流速为0.25 mL/min。采用电喷雾离子化源, 以多反应监测(MRM)方式分析, 正离子化进行检测。结果 碱性橙和碱性玫瑰精的线性范围为5~1000 μg/L, 相关系数良好。辣椒粉中碱性橙和碱性玫瑰精的检出限分别为2 μg/kg和0.5 μg/kg, 该方法在三个水平上添加回收率为88.1%~106.4%, 相对标准偏差为5.3%~11.7%。结论 本方法灵敏度高, 操作简单高效, 适合于辣椒粉中碱性橙和碱性玫瑰精的定量及确证分析。

英文摘要:

      Objective To develop a liquid chromatography-tandem mass spectrometry with solid phase dispersion for the determination of chrysoidine G and rhodamine B in paprika. Methods The sample was ultrasonically extracted from homogenized samples with acetonitrile, and cleaned up by dispersive ODS-C18 and PSA, then determined by electrospray ionization in positive mode using multiple reactions monitoring (MRM) finally. Results There was a good linear relationship in range of 5~1000 μg/L of chrysoidine G and rhoda-mine B. The limit of detection for chrysoidine G and rhodamine B was 2 μg/kg and 0.5 μg/kg. The recoveries were 88.1%~106.4% of three spiked levels, and RSDs were between 5.3%~11.7% (n=6). Conclusion This method is simple, effective and sensitive, and it is suitable for the determination and confirmation of chrysoidine G and rhodamine B in paprika.