高效液相色谱-串联质谱法测定保健食品中28种非法添加抗风湿类药物
Determination of 28 kinds of illegally added anti-rheumatic drugs in health food by high performance liquid chromatography tandem mass spectrometry method
羊银 1刘莹 1张瑞华 1柳溪 1张一楠 1李莹1
作者信息
- 1. 天津市食品安全检测技术研究院,天津 300308
- 折叠
摘要
目的 建立一种高效液相色谱-串联质谱法测定保健食品中抗风湿类药物含量的分析方法.方法 样品经超声提取和稀释后利用ZORBAX Eclipse Plus RRHD C18(3.0×150 mm,1.8 μm)色谱柱分离,通过流动相0.1％甲酸-5 mmol/L乙酸铵水溶液(A)-甲醇(B)梯度洗脱,多反应监测模式(multiple reaction monitoring,MRM)测定,外标法定量.结果 28种化合物在线性范围内线性关系良好,决定系数(R2)均≥0.99,检出限(limits of detection,LOD)为0.18～4.05 ng/mL;定量限(limits of quantitation,LOQ)为0.29～11.85 ng/mL;平均回收率介于62.1％～116.4％;平均相对标准偏差为1.1％～13.3％.结论 该方法可用于保健食品中非法添加抗风湿类药物的定性定量分析.
Abstract
Objective To develop a high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)method for the determination of 28 anti-rheumatic drugs in health food.Methods After ultrasonic extraction and dilution,the separation was achieved on a ZORBAX Eclipse Plus RRHD C18(3.0×150 mm,1.8 μm)column in a gradient elution mode with water(0.1％formic acid-5 mmol/L ammonium acetate)(A)and methanol(B),positive ion scan mode and a multiple reaction monitoring(MRM)mode were used to quantitatively determine the illegally added compounds by external standard method.Results The linear relationship of 28 compounds was good in the linear range,with determination coefficients(R2)≥0.99,the limits of detection(LODs)were 0.18-4.05 ng/mL,the limits of quantitation(LOQs)were 0.29-11.85 ng/mL,the average recoveries were 62.1％-116.4％,and the mean relative standard deviation were 1.1％-13.3％.Conclusion This method can be used for qualitative and quantitative analysis of illegally added anti-rheumatic drugs in health food.
关键词
抗风湿/非法添加物/液相色谱串联质谱法/保健食品Key words
Anti-rheumatic/Illegal additive/High performance liquid chromatography tandem mass spectrometry method/Health foods引用本文复制引用
基金项目
天津市市场监督管理委员会科技计划项目(2023-W31)
出版年
2024
NETL
NSTL
万方数据