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作 者:张秀尧[1] 蔡欣欣[1] 张晓艺[1] 李瑞芬[1]
机构地区:[1]温州市疾病预防控制中心,浙江温州325001
出 处:《色谱》2017年第11期1137-1144,共8页Chinese Journal of Chromatography
摘 要:采用在线净化-超高效液相色谱-三重四极杆/复合线性离子阱质谱(TF-UPLC-QTRAP MS)技术,建立了食品中吗啡、可待因、蒂巴因、罂粟碱、那可丁和原阿片碱6种罂粟壳标志物的快速确证检测方法。样品经0.10 mol/L盐酸提取、正己烷脱脂后,直接注入TF-UPLC-QTRAP MS进行分析。对影响净化的条件如TF-净化柱、流动相、洗脱溶液等条件进行了优化。确定以TurboFlow Cyclone MCX柱作为净化柱,Acquity BEH C_(18)柱为分析柱,甲醇-0.05%(体积分数)氨水溶液作为流动相,电喷雾正离子模式下多反应监测-触发增强子离子(MRM-IDA-EPI)扫描方式检测,以溶剂标准内标法定量。方法的检出限为0.05~0.5μg/kg,定量限为0.2~2μg/kg。平均加标回收率为81.1%~98.6%,相对标准偏差为2.9%~15.7%(n=6)。该方法灵敏、准确,适用于食品中非法添加罂粟壳的检测,已应用于实际样品的测定。A fast confirmation method was developed for the determination of the six markers of pericarpium papaveris,morphine,codeine,narcotine,papavarine,thebaine and protopine in foods, by TurboFlow online purification-ultra performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry (TF-UPLC-QTRAP MS). The sample was extrac-ted with 0. 10 mo^L HCl. After the procedure of removal of lipid with hexane,the extraction solution was analyzed by TF-UPLC-QTRAP MS. The main factors influencing the purification efficiency including TurboFlow column,mobile phase and elution solution were optimized. The six opium alkaloids were detected by positive electrospray ionization tandem mass spectrometry in the multiple reaction monitoring-information-dependent acquisition-enhanced product ion (MRM-IDA-EPI) mode,and quantified by solvent standard internal standard method. The limits of detection were 0. 05-0. 5 pg/kg and the limits of quantification were 0. 2-2 pg/kg for the six opium alkaloids. The recoveries were in the range of 81. 1%-98. 6% with the relative standard deviations ranging from 2. 9% to 15. 7% (n = 6). The method is sensitive and accurate,and has been successfully applied to the detection of pericarpium papaveris illegally added in foods.
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