摘要
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.
作者
宁霄
金绍明
董喆
赵云峰
曹进
NING Xiao;JING Shao-ming;DONG Zhe;ZHAO Yun-feng;CAO Jin(National Institute of Food and Drug Control,Beijing 100050,China;China national Center for Food Safety Risk Assessment,Beijing 100022,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2022年第5期821-830,共10页
Chinese Journal of Pharmaceutical Analysis
基金
“十三五”国家重点研发计划重点专项(2017YFC1601300)。
关键词
超高效液相色谱-串联质谱
非法添加
硝苯地平
去氢硝苯地平
去氢亚硝基硝苯地平
食品
保健食品
ultra performance liquid chromatography-tandem mass spectrometry
illegally adulterated
nifedipine
dehydro nifedipine
dehydronitroso nifedipine
food
health food