【摘要】 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。更多还原

【Abstract】 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 flowed 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 0.5～300 ng/g, with their detection limits(S/N=3) among 0.1～2 ng/g, the quantitative limits(S/N=10) 0.5～3 ng/g, the recoveries(20 ng/g, 200 ng/g) 82.0%～101.4%, the relative standard deviations(RSD, n=6) 1.4%～4.2%, the matrix effects(20 ng/g, 200 ng/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.更多还原