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目的建立快速、准确的HPLC-Q-TOF法测定降糖类中成药及保健食品中14种非法添加药物。方法样品采用50%乙腈提取,色谱柱为Thermo syncronis C18(150mm×4.6mm,5μm),流动相:0.1%甲酸-乙腈梯度洗脱,流速:0.3ml·min~(-1),柱温:30℃。采用ESI源,正离子扫描模式。结果 14种非法添加化合物在0.01~1μg·ml~(-1)范围内峰面积与浓度均呈良好的线性关系,r>0.998,回收率在78.0%~98.6%,RSD在2.3%~8.3%,检出限均在0.03~0.10μg·g~(-1)范围内。结论本方法快速准确,灵敏度高,能够同时满足对降糖类中成药及保健食品中14种非法添加药物的定性定量分析。
OBJECTIVE To establish a rapid and accurate HPLC-Q-TOF method for the determination of 14 kinds of illicitly added drugs in hypoglycemic Chinese medicines and health foods. Methods The sample was extracted with 50% acetonitrile, the column was Thermo syncronis C18 (150mm × 4.6mm, 5μm), the mobile phase was eluted with 0.1% formic acid and acetonitrile, the flow rate was 0.3ml · min -1, 30 ° C. Using ESI source, positive ion scan mode. Results The peak areas and concentrations of 14 compounds illegally added in the range of 0.01 ~ 1μg · ml ~ (-1) showed a good linear relationship with r> 0.998, recoveries ranged from 78.0% to 98.6% and RSD ranged from 2.3% to 8.3% , The detection limits are in the range of 0.03 ~ 0.10μg · g ~ (-1). Conclusion The method is rapid and accurate with high sensitivity and can meet the qualitative and quantitative analysis of 14 kinds of illicitly added drugs in hypoglycemic Chinese medicine and health food.