超高效液相色谱-串联质谱法测定食品及保健食品中硝苯地平、去氢硝苯地平和去氢亚硝基硝苯地平含量

Determination of nifedipine, dehydronifedipine and dehydronitroso nifedipine in food and health food by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法(ultraperformanceliquidchromatography-tandemmass spectrometry, UPLC-MS/MS)测定食品及保健食品中非法添加的硝苯地平及其降解产物去氢硝苯地平和去氢亚硝基硝苯地平含量的分析方法。方法样品用甲醇超声提取,经WatersAtlantisT3色谱柱(2.1mm×100mm,3μm)分离,以0.1%(V/V)甲酸水溶液-甲醇作为流动相,进行梯度洗脱。在正离子扫描条件下,采用多反应监测(multiple reaction monitoring, MRM)模式监测。结果硝苯地平、去氢硝苯地平和去氢亚硝基硝苯地平的浓度在2~100ng/mL范围内与峰面积线性均良好,相关系数(r)均在0.99以上。硝苯地平、去氢硝苯地平,去氢亚硝基硝苯地平在糖果、袋泡茶、奶粉、胶囊、颗粒、饮料等6种基质中50、125、1250μg/kg 3个水平下的加标回收率为76.3%~106.1%,相对标准偏差均未超过10%(n=6)。结论本方法简单、快速、灵敏度高,可满足食品及保健食品市场的监管和检验需求。

Objective To establish a method for the determination of nifedipine and its degradation products deshydronifedipine and deshydronitroso nifedipine content in food and health food by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). Methods Samples were extracted with methanol under ultrasonic condition, and separated on Waters Atlantis T3 chromatographic column(2.1 mm×100 mm, 3 μm). Gradient elution was carried out with 0.1%(V/V) formic acid aqueous solution and methanol as mobile phase. The determination was conducted in positive electrospray ionization mode under multiple reaction monitoring(MRM)mode. Results The linearity of difedipine, dehydronifedipine and dehydronitroso nifedipine were good in the range of 2-100 ng/mL, with correlation coefficients(r) all above 0.99. The recoveries of all components were 76.3%-106.1% with the relative standard deviations(RSDs) no more than 10%(n=6) at 3 spiked levels 50, 125 and 1250 μg/kg in candy, tea, milk powder, capsule, granule and drinks. Conclusion This method is specific, easy, fast, accuracy and sensitive, which can meet the needs of supervision and inspection of illegal added drugs in food and health products market.