摘要
目的:建立高效液相色谱串联质谱法(HPLC-MS/MS法)同时测定三高(高血糖、高血脂、高血压)人群用保健食品中45个违法添加的化学药物。方法:采用5 mmol·L~(-1)乙酸铵溶液(用甲酸调节pH至3.0)和乙腈,在Agilent Eclipse Plus C18柱(100 mm×2.1 mm,1.8μm)上进行梯度洗脱,流速为0.2 mL·min~(-1);质谱采用电喷雾离子源(ESI)正负离子模式将样品离子化,并用多反应监测(MRM)模式对45个化学药物进行测定。结果:45个化学药物在各自考察范围内线性良好,相关系数均大于0.995 0;平均回收率(n=3)为63.3%~129.5%(RSD:0.20%~9.9%),精密度和稳定性试验的RSD分别为0.50%~9.7%,1.0%~9.9%;正离子模式下检测下限为0.02~7 ng·g~(-1),负离子模式下检测下限为128 ng·g~(-1)。300批样品中共检出3批阳性样品,检出物分别是苯乙双胍、格列本脲、氢氯噻嗪和氨氯地平。结论:该HPLC-MS/MS法可用于测定三高人群用保健食品中45个违法添加的化学药物。
Objective:To establish an ultra-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for the simultaneous determination of 45 illegal addition chemical drugs in hyperglycemic,hyperlipidemic and hypertensive people's health foods.Methods:45 illegal addition components were well separated by the gradient elution of 5 mmol·L~(-1) ammonium acetate aqueous solution(adjust to pH 3.0 with formic acid)and acetonitrile on an Agilent Eclipse Plus C_(18)(100 mm×2.1 mm,1.8 μm)at a flow rate of 0.2 mL·min~(-1).MS detection was carried out by positive/negative electrospray ionization(ESI)mass spectrometer in multiple reaction monitor(MRM)mode.Results:The method validation showed good linarites with correlation coefficients(r~2)above 0.995 0 for all components.The mean recoveries ranged from 63.3% to 129.5%(RSD:0.20%-9.9%).The RSD values for precision were in the ranges of 0.50% to 9.7%,while those for stability were in the ranges of 1.0% to 9.9%. Meantime,the LOD values in positive mode were in the range of 0.02-7 ng·g~(-1),while the LOD was 128 ng·g~(-1) in negative mode.3 batches of positive samples were detected in 300 batches of samples,and the components were phenformin,glibenclamide,hydrochlorothiazide and mlodipine.Conclusion:This HPLCMS/MS method can be used for determination of 45 illegal addition components in hyperglycemic,hyperlipidemic and hypertensive people's health foods.
引文
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