UPLC-MS/MS法检测食品及保健食品中非法添加硝苯地平的研究

Determination of nifedipine illegally adulterated in food and health foods by UPLC-MS/MS

目的:建立UPLC-MS/MS同时检测食品及保健食品中非法添加硝苯地平及其2个降解产物去氢硝苯地平、去氢亚硝基硝苯地平的方法。方法:样品用含5%甲酸的乙腈水溶液超声提取,采用C_(18)色谱柱(2.1 mm×50 mm,1.8μm)分离,以2 mmol·L^(-1)甲酸铵-0.1%甲酸水溶液和乙腈为流动相,梯度洗脱,流速0.4 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3种化学成分在2~100μg·L^(-1)浓度范围内的线性关系良好,得到较好的分离度。低、中、高3个添加水平的平均回收率为90.9%~103.0%,RSD为1.2%~6.1%,各组分在各种基质中的检出限均低于0.05 mg·kg^(-1),定量限均低于0.1 mg·kg^(-1),并在5家实验室间进行了协同验证。结论:经方法学验证,所建立的分析方法可靠、灵敏、准确、简便,降低假阴性风险,适用于食品及保健食品中硝苯地平非法添加的快速筛查及定量分析。

Objective:To establish an UPLC-MS/MS method for simultaneous determination of nifedipine and its two degradation products(dehydro nifedipine and dehydronitroso nifedipine)added illegally in food and health food.Methods:Samples were extracted by acetonitrile aqueous solution containing 5%formic acid.The analysis was performed on C_(18)(50 mm×2.1 mm,1.8μm)column with gradient elution using a mobile phase of 0.1%aqueous formic acid(2 mmol·L^(-1)ammonium formate)and acetonitrile at 0.4 mL·min^(-1).Mass spectrometry acquisition was done in the positive ion mode and analytes were detected in the MRM mode.Results:Three chemical components could be separately well and have a good linear relationship in 2-100μg·L^(-1)range.The average recovery rates of low,medium and high concentration were 90.9%-103.0%with the RSD of 1.2%-6.1%.The detection limits and quantitation limits of each component in various matrices were lower than 0.05 mg·kg^(-1)and 0.1 mg·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 food health food.