超高效液相色谱-串联质谱法测定改善胃肠道功能类食品及中成药中非法添加的15种化学药物

Determination of 15 kinds of chemical drugs illegally added in foods for improving gastrointestinal function and Chinese patent medicines by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法测定改善胃肠道功能类食品(保健食品)及中成药中非法添加的15种化学药物的分析方法。方法样品用甲醇超声提取,经Waters Atlantis T_(3)色谱柱(2.1 mm×100 mm, 3μm)分离,以0.1%(V/V)甲酸水溶液-0.1%甲酸乙腈作为流动相,进行梯度洗脱。在正离子扫描条件下,采用多反应监测模式监测。结果尼扎替丁、西咪替丁、法莫替丁、艾普拉唑在10~100 ng/mL浓度范围内线性均良好(r>0.99),拉呋替丁、雷尼替丁、多潘立酮、兰索拉唑、奥美拉唑、莫沙必利、西沙必利、普芦卡必利、比沙可啶、替加色罗、酚酞在1~10ng/mL浓度范围内线性均良好(r>0.99)。15种化合物的加标回收率为87.7%~120.4%,精密度在0.6%~7.6%之间。结论本方法快速、灵敏,可用于改善胃肠道功能类食品(保健食品)和中成药中15种化学药物的快速筛查和定量测定。

Objective To establish a method for the determination of 15 kinds of drugs illegally added into foods(health foods) and Chinese traditional patent medicine for improving gastrointestinal function by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods The sample was ultrasonically extracted with methanol, and separated on a Waters Atlantis T_(3) column(2.1 mm×100 mm, 3 μm) using 0.1%(V/V) formic acid aqueous solution and 0.1% formic acid acetonitrile as the mobile phase for gradient elution. Under positive ion scanning conditions, multiple reaction monitoring(multiple reaction monitoring, MRM) mode was used for monitoring. Results Nizatidine, cimetidine, famotidine, ilaprazole had good linearity in the concentration range of 10-100 ng/mL(r>0.99), lafutidedin, ranitidine, domperidone, lansoprazole, omeprazole, mosapride, cisapride, prucalopride, bisacodyl, tegaserod,phenolphthalein had good linearity in the concentration range of 1-10 ng/m L(r>0.99). The spiked recoveries of 15 compounds were 87.7%-120.4% with precision between 0.6% and 7.6%. Conclusion This method is fast and sensitive, and can be used for rapid screening and quantitative determination of 15 drugs in foods(health foods) for improving gastrointestinal function and Chinese traditional patent medicines.