超高效液相色谱-串联质谱法检测豆制品中的碱性橙2

Determination of chrysoidine G in soy products by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  碱性橙2  豆制品  阳离子交换固相萃取柱  超高效液相色谱-串联质谱法

英文关键词:chrysoidine G  soy products  cation exchange solid phase extraction column  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱法测定豆制品中碱性橙2含量的方法。方法 样品均质后, 用0.4%乙酸-20 mmol/L乙酸铵+乙腈(1:1, V:V)超声提取, 经混合型阳离子交换固相萃取柱净化, 氮吹、50%乙腈复溶后上机。采用0.1%甲酸-10 mmol/L甲酸铵(A)和乙腈(B)作为流动相进行梯度洗脱。质谱采用多反应监测模式对碱性橙2的定量离子和定性离子进行监测。结果 碱性橙2在0.1~10.0 ng/mL线性范围内线性关系良好, 相关系数大于0.999。碱性橙2在4.0、8.0和40.0 μg/kg添加水平的回收率为86.2%~106.2%, 相对标准偏差不超过3.6% (n=6), 方法定量限为4.0 μg/kg。结论 该方法准确、灵敏, 适合豆制品中碱性橙2的测定分析。

英文摘要:

      Objective To establish a method for the determination of chrysoidine G in soy products by ultra performance liquid chromatography-tandem mass spectrometry. Methods After homogenization, the sample was extracted by 0.4% acetic acid -20 mmol/L ammonium acetate+acetonitrile (1:1, V:V), purified by mixed cation exchange solid phase extraction column and blown-dry by nitrogen. Then it was dissolved by 50% acetonitrile and separated on a reversed phase using 0.1% formic acid -10 mmol/L ammonium formate solution (A) and acetonitrile solution (B) as mobile phase for gradient elution program. The quantitative and qualitative ions of chrysoidine G were monitored by mass spectrometry with multiple reaction monitoring mode. Results Chrysoidine G had a good linear relationship in the linear range of 0.1 to 10.0 ng/mL, the correlation coefficient was greater than 0.999. The recoveries were ranged from 86.2% to 106.2% for the chrysoidine G with 3 spiked levels of 4.0, 8.0 and 40.0 μg/kg. The relative standard deviations were no more than 3.6% (n=6), and the limits of quantitation for chrysoidine G was 4.0 μg/kg. Conclusion The proposed method is accurate and sensitive, which is suitable for detecting chrysoidine G in soy products.