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目的建立食品中罂粟碱、吗啡、那可丁、可待因和蒂巴因等5种生物碱同时测定的固相萃取-超高效液相色谱-串联质谱法(SPE-UPLC-MS/MS)。方法样品经乙腈-0.1 mol/L盐酸(1∶4,V/V)提取,MCX固相萃取柱净化,采用BEH HILIC色谱柱(2.1 mm×100 mm,1.7μm),以乙腈-10 mmol/L乙酸铵-0.1%甲酸水溶液作为流动相,梯度洗脱,采用电喷雾电离源正离子模式(ESI+)在多反应监测(MRM)模式下分析检测。吗啡和可待因以同位素标记的内标定量,罂粟碱、那可丁和蒂巴因以外标法定量。结果各化合物在0.5μg/L~80.0μg/L范围内均呈现良好的线性关系,相关系数均>0.999,5种化合物的检出限为0.4μg/kg~1.0μg/kg,添加回收率为85.8%~103.5%,相对标准偏差为2.3%~11.6%。结论该方法具有操作简便,灵敏度高,重现性好等特点,可满足食品中5种生物碱同时检测的要求。
OBJECTIVE To establish a solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS / MS) for the simultaneous determination of five alkaloids, papaverine, morphine, . Methods The samples were extracted with acetonitrile-0.1 mol / L hydrochloric acid (1: 4, V / V) and cleaned up by MCX solid phase extraction. The samples were eluted with BEH HILIC (2.1 mm × 100 mm, L ammonium acetate-0.1% formic acid aqueous solution as a mobile phase, gradient elution, and electrospray ionization source positive ion mode (ESI +) in multiple reaction monitoring (MRM) mode. Morphine and codeine were quantified using an isotope-labeled internal standard. Papaverine, nardocin, and thebaine were quantified by external standards. Results The results showed that all the compounds showed good linearity in the range of 0.5μg / L to 80.0μg / L with the correlation coefficients> 0.999. The detection limits of the five compounds ranged from 0.4μg / kg to 1.0μg / kg. The recoveries were 85.8% ~ 103.5%, the relative standard deviation was 2.3% ~ 11.6%. Conclusion The method has the characteristics of simple operation, high sensitivity and good reproducibility, which can meet the requirements of simultaneous detection of five alkaloids in food.