改良QuEChERS-超高效液相色谱-串联质谱法快速测定减肥食品中19种违禁药物

Rapid determination of 19 kinds of prohibit drugs in diet foods by improved QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  减肥食品  QuEChERS  违禁药物  快速筛查

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  diet food  QuEChERS  prohibit drugs  rapid screening

中文摘要:

      目的 建立改良QuEChERS-超高效液相色谱-串联质谱法, 对减肥食品中19种违禁药物进行快速筛查。方法 样本经1%甲酸-甲醇提取, 超声水浴20 min助提, 提取液经含有N-丙基乙二胺(primary secondary amine, PSA)、C18、石墨化炭黑(graphitized carbon black, GCB)吸附剂的QuEChERS小柱净化, 以0.1%甲酸-水/甲醇为流动相, C18色谱柱分离, 由超高效液相色谱-串联质谱法在多反应监测模式(multiple reaction monitoring, MRM)下进行分析。结果 19种违禁药物仪器总分析时长仅为9.5 min, 各组分保留时间在0.77~7.31 min之间, 且色谱图峰型良好。各组分在5~200 μg/L的线性范围内相关系数(r2)均大于0.99, 检出限为0.7~105.5 μg/kg, 定量限为2.2~312.5 μg/kg, 3个加标浓度(200、40、8 μg/kg)下19种违禁药物回收率为64.50%~128.75%, 相对标准偏差(relative standard deviations, RSDs)均小于10% (n=6)。结论 该方法具有操作简便、仪器维护成本低、分析快速、回收率高、基质干扰小等优点, 适用于减肥食品中多种违禁药物的快速筛查。

英文摘要:

      Objective To establish a rapid method for the screening of 19 kinds of prohibit drugs in diet foods by improved QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with 1% formic acid-methanol solution, assisted by ultrasonic water bath for 20 min, the supernatant was purified by QuEChERS cartridges containing adsorbents of primary secondary amine (PSA), C18, graphitized carbon black (GCB), separated by C18 column with 0.1% formic acid-water and methanol as mobile phases, the analysis was performed by ultra performance liquid chromatography-tandem mass spectrometry in multiple reaction monitoring (MRM) mode. Results The total analysis time of 19 kinds of prohibit drugs was only 9.5 min, and the retention times were between 0.77 and 7.31 min, the peak shape of each component chromatogram was good. The correlation coefficient (r2) of each component in the linear range of 5?200 μg/L was greater than 0.99, the limits of detection were 0.7?105.5 μg/kg, the limits of quantitation were 2.2?312.5 μg/kg, the recoveries at the spiked concentrations of 200, 40, 8 μg/kg were 64.50%?128.75%, and the relative standard deviations (RSDs) were less than 10% (n=6). Conclusion This method has the advantages of simple operation, low instrument maintenance cost, rapid analysis, high recovery rate, and low matrix interference, which is suitable for the rapid screening of multiple prohibit drugs in diet food.