超高效液相色谱-串联质谱法检测多基质保健食品中27种非法添加降糖类化合物

Determination of 27 kinds of anti-diabetic compounds illegally in different kinds of health food by ultra-performance liquid chromatography- tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  保健食品  降糖化合物  非法添加

英文关键词:ultra-performance liquid chromatography-tandem mass spectrometry  health food  anti-diabetic compounds  illegally additives

中文摘要:

      目的 建立超高效液相色谱-三重四极杆质谱法检测保健食品中27种降糖类非法添加化合物的分析方法。方法 4种不同基质保健品样品经甲醇超声提取后, 采用Waters XBridge Amide色谱柱(2.1 mm× 100 mm, 3.5 μm), 以5 mmol/L甲酸铵水溶液和5 mmol/L甲酸铵乙腈作为流动相进行梯度洗脱, 分离苯乙双胍、二甲双胍、伏格列波糖、阿卡波糖、丁二胍5种化合物; 采用Waters CORTECS T3色谱柱(2.1 mm×100 mm, 2.7 μm), 以0.1%甲酸水溶液和乙腈作为流动相进行梯度洗脱, 分离维达列汀、罗格列酮、西他列汀、吡格列酮等22种化合物; 环格列酮采用电喷雾离子化负离子模式, 其他26种化合物采用电喷雾离子化正离子模式, 以多反应监测方式进行检测。结果 伏格列波糖、阿卡波糖、达格列净、卡格列净、曲格列酮、环格列酮6种化合物在0.25~12.5 μg/mL范围内线性关系良好, 其他21种化合物在5~250 ng/mL范围内线性关系良好, 线性相关系数r均大于0.99; 27种化合物检出限为1~1000 μg/kg; 在低、中、高3水平加标, 其回收率为70%~120%, 相对标准偏差为0.7%~10% (n=6)。结论 本方法快速、灵敏、高效、准确, 适用范围广, 可用于保健食品中降糖类化合物的高通量检测。

英文摘要:

      Objective To establish a method for determination of 27 kinds of anti-diabetic compounds illegally in health foods by ultra-performance liquid chromatogtaphy-triple quadrupole mass spectrometry. Methods Four different kinds of health foods were processed with methanol by ultrasonic extraction. Phenformin and other 5 compounds were seperated by Waters XBridge Amide column (2.1 mm×100 mm, 3.5 μm) with 5 mmol ammonium formate aqueous solution–5 mmol ammonium formate acetonitrile as mobile phases for gradient elution. The other 22 compounds such as vildagliptin, rosiglitazone, sitagliptin, pioglitazone, etc, were seperated by Waters CORTECS T3 column (2.1 mm×100 mm, 2.7 μm) with 0.1% formic acid aqueous solution-acetonitrile as mobile phases for gradient elution. Ciglitazone was detected by electrospray ion souce in negative mode, and the other 26 compounds were detected by electrospray ion souce in positive mode with multiple reaction monitoring mode. Results Voglibose, acarbose, dagliquin, cagliquin, triglazone and cycloglazone showed good linear relationship in the range of 0.25? 12.5 μg/mL The other 21 compounds had good linear relationships in the range of 5?250 ng/mL, and the linear correlation coefficients r were all greater than 0.99. The limits of detections of 27 compounds were 1?1000 μg/kg. The recoveries of the 27 compounds were 70%?120% at low, medium and high levels, and the relative standard deviations were 0.7%?10% (n=6). Conclusion This method is rapid, efficient and accurate, which can be widely appliacated in the detection of anti-diabetic compounds illegally in diffierent kinds of health food matrices.