CAJ | 학술논문

建立了高效液相色谱-三重四极杆线性离子阱质谱测定火锅料中吗啡、可待因、蒂巴因、罂粟碱、那可丁等5种生物碱残留的确证方法。样品采用稀盐酸加热提取，正己烷除脂，阳离子混合机理固相萃取柱净化，5％氨化乙酸乙酯-甲醇洗脱，PAK ST色谱柱分离，5 mmol／L乙酸铵甲醇溶液-10 mmol／L 乙酸铵水溶液（ pH 3.6）作为流动相洗脱，电喷雾正离子模式下多反应监测同步增强子离子在线全扫描（ EPI）。在该实验条件下，5种生物碱的 LOD在0.05~0.5μg／kg之间，增强型子离子全扫描水平限和 LOQ 在0.2~2μg／kg 之间，方法回收率为64.2％~110.6％，RSD为4.2％~12.5％。阳性样品的定性确证需采用其子离子全扫描质谱图与标准图库中子离子质谱图检索匹配。经测定多种火锅料，表明本方法操作简单、测定结果准确，可用于火锅料中5种生物碱残留的阳性结果确证分析。
건립료고효액상색보-삼중사겁간선성리자정질보측정화과료중마배、가대인、체파인、앵속감、나가정등5충생물감잔류적학증방법。양품채용희염산가열제취，정기완제지，양리자혼합궤리고상췌취주정화，5％안화을산을지-갑순세탈，PAK ST색보주분리，5 mmol／L을산안갑순용액-10 mmol／L 을산안수용액（ pH 3.6）작위류동상세탈，전분무정리자모식하다반응감측동보증강자리자재선전소묘（ EPI）。재해실험조건하，5충생물감적 LOD재0.05~0.5μg／kg지간，증강형자리자전소묘수평한화 LOQ 재0.2~2μg／kg 지간，방법회수솔위64.2％~110.6％，RSD위4.2％~12.5％。양성양품적정성학증수채용기자리자전소묘질보도여표준도고중자리자질보도검색필배。경측정다충화과료，표명본방법조작간단、측정결과준학，가용우화과료중5충생물감잔류적양성결과학증분석。
A confirmative method was developed for determining five poppy alkaloids including morphine,codeine,papaverine,tibane,noscapine in chafing dish ingredients by high perform-ance liquid chromatography coupled with triple quadrupole linear ion trap mass spectrometry (HPLC-Q Trap MS). The sample was extracted with dilute HCl solution under heating condi-tion. The removal of lipid procedure was performed with hexane. The purification was carried out on a mixed-cation solid-phase extraction column( MCX)and ethyl acetate-methanol contai-ning 5% aqueous ammonia was used for elution. A PAK ST column was used to separate the analytes,and 5 mmol/L ammonium acetate methanol and 10 mmol/L ammonium acetate( pH 3. 6)were used as mobile phases. The five alkaloids was detected in the positive mode simulta-neously by multiple reaction monitoring ( MRM ) and online enhanced product ion full scan ( EPI). The LODs were 0. 05-0. 5 μg/kg and the LOQs were 0. 2-2 μg/kg for the five poppy alkaloids. The overall recoveries of the method varied from 64. 2% to 110. 6%,and the RSD were between 4. 2% and 12. 5%. The EPI mass spectra of positive samples were searched through standard library for qualitative confirmation. The detection of real hot pot material sam-ples showed this method can be used for the simple and accurate determination of the five pop-py alkaloid residues in chafing dish.