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C18色谱柱(2.1 mm×50 mm,1.8 μm)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2～100 μg·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 C18(50 mm×2.1 mm,1.8 μm)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 2-100 μg·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.
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