HPLC-MS/MS法同时快速检测清咽类保健食品中添加的5个化学成分的方法

Simultaneous determination of five chemical compositions in health food by high performance liquid chromatography-tandem mass spectrometry

目的:建立HPLC-MS/MS法同时快速检测保健食品中非法添加的5个化学成分(沙丁胺醇、土霉素、磺胺甲噁唑、盐酸二氧丙嗪和枸橼酸喷托维林)的方法。方法:样品用甲醇溶解,采用ECLIPSE PLUS-C18色谱柱(2.1 mm×50 mm,1.8μm)分离,以10 mmol·L-1甲酸铵-含0.1%甲酸溶液和乙腈为流动相,梯度洗脱,流速0.2 mL·min-1,采用电喷雾离子源(ESI)正离子模式,多反应监测(MRM)进行检测。结果:所测5个非法添加化学成分在一定范围内呈良好的线性关系,得到较好的分离度。低、中、高3个添加水平的平均回收率为89.0%~105.2%,RSD为0.49%~3.6%,沙丁胺醇、土霉素、磺胺甲噁唑、盐酸二氧丙嗪和枸橼酸喷托维林的检测下限分别为0.62、12、8.3、0.55和0.72μg·kg-1。结论:经方法学验证,所建立的分析方法可靠、灵敏、准确,可用于清咽类保健食品中非法添加的5个化学成分同时定性和定量分析。

Objective:To establish an HPLC-MS/MS method for simultaneous determination of five chemical compositions(salbutamol,oxytetracycline,sulfamethoxazole,promethazine hydrochloride,pentoverine citrate)added illegally in health food.Methods:Samples were extracted by methanol.The analysis was performed on ECLIPSE PLUS-C18(50 mm×2.1 mm,1.8μm)column with gradient elution using a mobile phase of 0.1%aqueous formic acid(10 mmol·L-1 ammonium formate)and acetonitrile at 0.2 mL·min-1.Mass spectrometry acquisition was done in the positive ion mode and analytes were detected in the MRM mode.Results:Five illegally added chemical components could be separately well and have a good linear relationship in a certain range.The average recovery rates of low,medium and high concentration were 89.0%-105.2%with the relative standard deviation(RSD)of 0.49%-3.6%.The detection limit of salbutamol,oxytetracycline,sulfamethoxazole,promethazine hydrochloride,pentoverine citrate was 0.62,12,8.3,0.55 and 0.72μg·kg-1,respectively.Conclusion:The developed method verified by the methodology is precise,sensitive,accurate,which therefore can be applied for the analysis of illegally added in health food.