液液萃取-超高效液相色谱-串联质谱法测定常见食用植物油中5种鸦片生物碱

目的建立酸化甲醇(pH=3)液液萃取-超高效液相色谱-串联三重四极杆质谱(UPLC-MS/MS)测定常见食用植物油中5种鸦片生物碱吗啡、可待因、蒂巴因、罂粟碱、那可汀的检验方法。方法样品加入正己烷摇匀后用酸化甲醇(pH=3)提取,BEH C18色谱柱分离,乙腈(0.01%甲酸)-水(0.01%甲酸+0.05%氨水,体积比)梯度洗脱,电喷雾离子源正离子(ESI+)及多反应监测模式检测。结果结果显示5种待测成分在0.5~300ng/g范围内线性关系良好;方法检出限(S/N=3)在0.1~2ng/g间、定量限(S/N=10)在0.5~3ng/g间;回收率(20ng/g,200ng/g)在82.0%~101.4%间,相对标准偏差(RSD,n=6)为1.4%~4.2%,基质效应(20ng/g,200ng/g)在-5.3%~5.8%间,日间精密度为2.8%~6.7%。结论本方法前处理简单、耗时短,溶剂使用量少,灵敏度高,适合大批量常见食用植物油中5种鸦片生物碱的同时检测。

Liquid-liquid Extraction Combined with UPLC-MS/MS to Simultaneously Determine 5 Kinds of Opium Alkaloids in Common Edible Vegetable Oils

Objective To set up a method for determination of 5 opium alkaloids(noscapine,papaverine,thebaine,codeine,morphine)illegally adulterated into common edible vegetable oils through liquid-liquid extraction(LLE)combined with ultrahigh performance liquid chromatography-tandem triple quadrupole mass spectrometry(UPLC-MS/MS).Methods The seized samples were added of n-hexane and shaken to be homogenized,followed to extract with acidified methanol(pH=3).The extracted compounds were separated through a BEH C18 column being fl owed with the mobile phase of acetonitrile(0.01%formic acid)-hydrated mixture(0.01%formic acid,0.05%ammonia water,V/V)for gradient elution,with the eluted substances being detected under electrospray positive ionization(ESI+)plus multi-reaction monitoring(MRM)mode.Results The 5 targeted-to-detect compounds were revealed of good linear relationship in the range of 0.5~300ng/g,with their detection limits(S/N=3)among 0.1~2ng/g,the quantitative limits(S/N=10)0.5~3ng/g,the recoveries(20ng/g,200ng/g)82.0%~101.4%,the relative standard deviations(RSD,n=6)1.4%~4.2%,the matrix effects(20ng/g,200ng/g)-5.3%~5.8%,and the inter-day precisions 2.8%~6.7%.Conclusions The method is of simple pretreatment,short time consumption,less solvent usage and high sensitivity,suitable for simultaneous determination of 5 kinds of opium alkaloids in common edible vegetable oils.