UPLC-MS/MS法同时测定中成药和保健食品中非法添加治疗高尿酸血症类药物

Determination of hyperuricemia drugs for treatment illegally added in Chinese patent medicines and health foods by UPLC-MS/MS

建立超高效液相色谱-串联质谱法同时检测中成药和保健食品中非法添加的7种治疗高尿酸血症类药物的方法。色谱柱为ACQUITY UPLC?BEH C18(2.1 mm×100 mm,1.7μm),以0.2%甲酸水溶液-乙腈(流速为0.3 mL/min)为流动相梯度洗脱;质谱采用电喷雾离子源(ESI),正离子多反应监测(MRM)模式进行定性定量分析。结果表明,7种治疗高尿酸血症类药物在相应的质量浓度范围内线性关系良好,相关系数均大于0. 995,在低、中、高3个加标水平下的平均回收率为95.49%~104.87%,RSD为1.40%~3.44%,检出限为0.01~0.30μg/kg,定量限为0.04~1.00μg/kg,6批样品中有1批样品检出了非法添加的化学物质。该方法前处理简单,灵敏度高,结果准确,适用于中成药和保健食品中7种治疗高尿酸血症类药物的同时快速定性定量分析。

To establish a method for simultaneous detection of 7 hyperuricemia drugs for treatment illegally added to Chinese patent medicines and health foods by UPLC-MS/MS.The samples were extracted from samples with mobile phase,the column was a ACQUI⁃TY UPLC®BEH C18(2.1 mm×100 mm,1.7μm),a gradient elution with the mobile phase of 0.2%formic acid aqueous solution and acetonitrile solution at a flow rate of 0.3 mL/min.The compounds were detected by electrospray ion source in positive mode with multi⁃ple reaction monitoring(MRM)mode.The results showed that all the 7 hyperuricemia drugs for treatment with showed good linearity in their reasonable ranges,and the correlation coefficients were greater than 0.995.The average recoveries of low,medium and high concentrations ranged between 95.49%and 104.87%,and the relative standard deviations were 1.40%~3.44%.The LODs were 0.01~0.30μg/kg and LOQs were 0.04~1.00μg/kg.Illegal added chemical drugs were found in 1 of the 6 tested practical samples.With the advantages of simple pre-processed,high sensitivity and accurate results,the method can be used in determination of 7 hyperuricemia drugs for treatment in Chinese patent medicine and health foods.