分散固相萃取-超高效液相色谱-串联质谱法测定马铃薯中的抑芽丹

Determination of maleic hydrazide in potato by ultra performance liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction

中文关键词:  超声提取  分散固相萃取  超高效液相色谱-串联质谱法  马铃薯  抑芽丹

英文关键词:ultrasound extraction  dispersive solid phase extraction  ultra performance liquid chromatography- tandem mass spectrometry  potato  maleic hydrazide

中文摘要:

      目的 建立超声提取-分散固相萃取-超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)法测定马铃薯中的抑芽丹。方法 对样品的前处理方法及UPLC-MS/MS分析条件进行优化, 样品经乙腈提取、超声、分散固相萃取净化, 多反应监测模式(multiple reaction monitoring, MRM)进行测定。结果 抑芽丹在0.03~50.0 mg/kg范围内均呈良好的线性关系, 相关系数为0.9995; 检出限(S/N=3)为0.01 mg/kg, 定量限(limit of quantification, LOQ, S/N≥10)为0.03 mg/kg; 在加标量为0.01、0.1、50 mg/kg下, 回收率为83.7%~92.1%, 相对标准偏差为0.8%~4.9%。结论 该法简便、快速、结果准确可靠、灵敏度高, 可消除马铃薯中复杂基质的干扰, 适用于马铃薯中抑芽丹的测定。

英文摘要:

      Objective To establish a method for determination of maleic hydrazide in potato by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with dispersive solid phase extraction. Methods The sample pretreatment method and the analysis conditions of instruments were optimized. Samples were extracted by acetonitrile, and purified by ultrasonic and dispersive solid phase extraction, and then determined under multiple reaction monitoring (MRM) mode. Results In the range of 0.03-50.0 mg/kg, the maleic hydrazide showed a good linear relationship with the correlation coefficient of 0.9995. The limit of detection (S/N=3) was 0.01 mg/kg, and limit of quantification was 0.03 mg/kg (S/N≥10). At the spiked levels of 0.01, 0.1, and 50 mg/kg, the recoveries were 83.7%-92.1%, and the relative standard deviations were 0.8%-4.9%. Conclusion The method is simple, rapid, accurate and reliable with high sensitivity, and can eliminate the interference of complex substrates in potato, which is suitable for the determination of maleic hydrazide in potatoes.