同位素内标-超高效液相色谱-串联质谱法测定水产制品中9种甜菊糖苷类甜味剂

Determination of 9 kinds of stevioside compounds in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry with isotope internal standard

中文关键词:  内标法  水产制品  甜菊糖苷  高效液相色谱-串联质谱法

英文关键词:internal standard method  aquatic products  stevioside compounds  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 采用同位素内标法结合高效液相色谱-串联质谱法测定水产制品中9种甜菊糖苷类甜味剂的方法。方法 样品经甲醇水溶液(1:1, V:V)提取, CSH C18色谱柱分离, 梯度洗脱。使用电喷雾负离子模式, 以多反应监测模式采集, 内标法定量。结果 9种甜菊糖苷类甜味剂在0.1~100.0 ng/mL范围内线性关系良好, 检出限为2.0 μg/kg, 定量限为5.0 μg/kg。低、中、高3个浓度加标回收试验, 回收率为90.16%~103.69%, 相对标准偏差为2.24%~6.38%。采用该方法对水产制品进行分析, 检出率为12%。结论 该方法简便高效, 具有较高的准确度和灵敏度, 适用于水产制品中9种甜菊糖苷类甜味剂的测定。

英文摘要:

      Objective To establish a method for the determination of 9 kinds of stevioside compounds in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry with isotope internal standard. Methods The sample was extracted with methanol aqueous solution (1:1, V:V), separated on a CSH C18 chromatographic column, and eluted with a gradient. The sample was analyzed in multiple reaction monitoring mode using electrospray negative ionization mode and quantified by internal standard method. Results The 9 kinds of stevioside compounds showed good linear relationships in the range of 0.1–100.0 ng/mL. The limits of detection were 2.0 μg/kg, and the limits of quantitation were 5.0 μg/kg. The spiked recoveries of the method at low, medium and high spiked levels showed that the recoveries were in the range of 90.16%–103.69% with the relative standard deviations of 2.24%–6.38%. The method was used to analyze aquatic products, with a detection rate of 12%. Conclusion The method is simple, efficient, and highly accurate and sensitive, making it suitable for the determination of 9 kinds of stevioside compounds in aquatic products.