超高效液相色谱-串联质谱测定改善胃肠功能类保健食品中.docVIP

超高效液相色谱-串联质谱测定改善胃肠功能类保健食品中 添加的10种化学药物* 赵超群1，李樱红2，罗金文1,2 ** 浙江工业大学，杭州 310014；2. 浙江省食品药品检验研究院，杭州 310004） 摘要 目的：建立同时测定改善胃肠功能类保健食品中10种非法添加物含量的超高效液相色谱－串联质谱分析方法。方法: 采用Zorbax SB-C18（2.1mm×100 mm，1.8 μm）色谱柱，0.1%乙酸（含20 mmol·L-1乙酸铵）和甲醇为流动相（梯度洗脱），柱温35 ℃，流速0.2 mL·min-1，质谱条件为电喷雾电离源（ESI+），以多重反应监测（MRM）方式进行检测。喷雾电压为4 kV，辅助气温度为200 ℃，辅助气流量为14 L·min-1，鞘气温度为350 ℃，鞘气流量为11 L·min-1。结果: 10种药物在定量限到250倍定量限范围内有良好的线性关系，平均回收率（n=15）为86.9%~113%，检测限为0.02～0.4 ng·mL-1， RSD均小于5%（n=6），40批保健食品中检出4批阳性样品。结论: 该方法专属、灵敏、准确，可用于测定改善胃肠功能类保健食品中10种非法添加物。 关键词: 超高效液相色谱－串联质谱；多重反应监测；胃肠功能类保健食品；非法添加；含量测定 中图分类号：R917 文献标识码：A 文章编号：0254-1793（2014） Determination of 10 compounds adulterated in health food with improving gastrointestinal function by UPLC-MS/MS Abstract Objective: To establish an UPLC－MS/MS method for simultaneous determination of 10 compounds illegally adulterated in Health food with improving gastrointestinal function. Methods: The separation and analysis was performed on a Zorbax SB C18 column (2.1 mm×100 mm, 1.8 μm). The mobile phase consisted of 0.1% acetic acid containing 20 mmol·L-1 ammonium acetate and methanol (Gradient elution). The column temperature was set at 35 ℃ with flow rate of 0.2 mL·min-1．Electrospray ionization(ESI) source was applied and operated in the positive mode. Multiple reaction monitoring (MRM) mode was used to quantify the 10 compounds. Spray voltage was set at 4 kV. Auxiliary gas temperature was 200 ℃ and auxiliary gas flow rate was 14 L·min－1; Sheath gas temperature was 350 ℃ and sheath gas flow rate was 11 L·min-1. Results: The assay linearity of the 10 compounds illegally adulterated was confirmed over 1-250 times of the limit of quantification. The average recoveries( n=15) were 86.9%-113% ， the detection limits were 0.02-0.4 ng·mL-1and the relative standard deviation was less than 5%( n = 6). 40 batchs health food were tested. Phenolphthalein and sibutramine were found in 4 batchs of health food.Conclusion: The established method is proved to be specific，sensitive and