摘要
建立了超高效液相色谱-串联质谱(UPLC-MS/MS)联用法检测火锅底料中吗啡、可待因、那可丁、罂粟碱、蒂巴因5种生物碱残留的分析方法。样品经含0.2%甲酸的乙腈提取,PRi ME HLB固相萃取小柱快速净化,ACQUITY BHE C18色谱柱(1.7μm,2.1 mm×50 mm)分离,以p H 8.0氨水溶液和乙腈作为流动相,梯度洗脱,经电喷雾正离子(ESI+)模式电离及多反应监测(MRM)测定目标化合物,采用基质标准溶液曲线法定量分析。结果表明,吗啡、可待因的线性范围为0.25~100μg/L,蒂巴因的线性范围为0.05~100μg/L,那可丁、罂粟碱的线性范围为0.05~10μg/L,相关系数均大于0.999。5种生物碱的检出限为0.9~4.5μg/kg,定量下限为3.0~15.0μg/kg;在1、5、10μg/kg(吗啡和可待因为5、25、50μg/kg)3个加标水平下的回收率为70.7%~109.6%,相对标准偏差小于11%。该方法操作快速简单、灵敏度高,适用于火锅底料中罂粟壳生物碱残留的定性与定量分析。
A method of ultra performance liquid chromatography-tandem mass spectrometry （UPLC- MS/MS ） was developed for the simultaneous determination of 5 alkaloids residues of opium poppy in hot pot soup,including morphine,codeine,thebaine,papaverine and narcotine.The samples were extracted with acetonitrile containing 0.2 % fomic acid,and then analyzed by UPLC-MS/MS.The separation was carried out using a Waters ACQUITY UPLC TM BHE C 18 （1.7 μm,2.1 mm×50 mm ） column by gradient elution with ammonia solution （pH 8.0 ） and acetonitrile as mobile phases at a flow rate of 0.3 mL/min.The five alkaloids were determined in electrospray positive ionization （ESI ＋ ） mode under multiple reaction monitoring （MRM ）,and the analytes were quantified by the matrix-matched standard solution.Under the optimized detection conditions,the calibration curves are linear in the ranges of 0.25-100 μg/L for morphine and codeine,0.05-100 μg/L for thebaine,and 0.05-10 μg/L for papaverine and narcotinum,respectively,with correlation coefficients all more than 0.999.The limits of detection （LODs ） and quantitation （LOQs ） were in the ranges of 0.9-4.5 μg/kg and 3.0-15.0 μg/kg,respectively.The average recoveries at the spiked levels of 1,5,10 μg/kg （5,25,50 μg/kg for morphine and codeine ） ranged from 70.7 % to 109.6 % ,with relative standard deviations （RSDs ） not more than 11 % .This method is simple and sensitive,and is suitable for the determination and confirmation of five alkaloids residues of opium poppy illegally added in hot pot soup.
作者
李兴根
乔勇升
陈伟
冯寅洁
朱渊
胡慧
LI Xing-gen;QIAO Yong-sheng;CHEN Wei;FENG Yin-jie;ZHU Yuan;HU Hui(Taizhou Institute of Product Quality Supervision and Inspection,Taizhou 225300,China;Taizhou Institute for Food and Drug Control,Taizhou 225300,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2018年第4期446-451,共6页
Journal of Instrumental Analysis
关键词
固相萃取
超高效液相色谱-串联质谱(UPLC-MS/MS)
罂粟壳
罂粟碱
吗啡
火锅底料
solid phase extraction （SPE ）
ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS ）
poppy husk
papaverine
morphine
hot pot soup
