超高效液相-串联质谱法测定食品中罂粟壳成分

Determination of Pericarpium Papaveris in food by ultra high performance liquid chromatography-tandem mass spectrometry

中文关键词:  罂粟壳  罂粟碱  吗啡  前处理方法  液相色谱质谱联用法

英文关键词:Pericarpium papaveris  papaverine  morphine  pretreatment method  liquid chromatography-mass spectrometry

中文摘要:

      目的 建立超高效液相-串联质谱法测定食品中罂粟壳成分的分析方法。方法 罂粟壳经乙腈提取后, 经PCX固相萃取柱净化, 选择BEH HILIC柱(粒径1.7 μm, 2.1 mm×100 mm), 以含0.1%甲酸的10 mmol/L乙酸铵溶液和甲酸乙腈溶液(0.1%)作为流动相进行梯度洗脱, 在0.3 mL/min流速下, 以多反应监测(multiple reaction monitoring, MRM)扫描模式进行检测, 外标法定量。结果 吗啡、可待因在25~250 μg/kg添加浓度范围内, 回收率为68.30~80.81%。罂粟碱、那可丁、蒂巴因在0.5~2.5 μg/kg添加浓度范围内, 回收率为68.34%~78.91%。本方法罂粟碱、那可丁、蒂巴因、吗啡和可待因定量限分别为0.5、0.5、0.5、25、25 μg/kg。结论 该方法简便、快速、可靠, 可用于各种食品中罂粟壳生物碱的快速筛查与确证。

英文摘要:

      Objective To establish a method of ultra-high performance liquid chromatography-tandem mass spectrometry for the determination of Pericarpium papaveris in food. Methods After extraction with acetonitrile, Pericarpium papaveris was purified by PCX solid phase extraction column. The liquid was performed on BEH HILIC (1.7 μm, 2.1 mm×100 mm) with gradient elution of 10 mmol/L ammonium acetate solution (containing 0.1% formic acid) and acetonitrile (containing 0.1% formic acid), and the flow rate was 0.3 mL/min. The sample was detected in multiple reaction monitoring (MRM) scan mode, and quantified by external standard method. Results The recoveries rate of morphine, codeine in the range of 25?250 μg/kg was 68.30%?80.81%. The recoveries rate of papaverine, nacodin and thebaine in the range of 0.5?2.5 μg/kg was 68.34%?78.91%. The quantitative limits of papaverine, nacodin, thebaine, morphine and codeine of the method were0.5, 0.5, 0.5, 25, 25 μg/kg. Conclusion This method is simple, fast and reliable, which can be used for rapid screening and confirmation of poppy shell alkaloids in various foods.