同位素内标-多反应监测同步在线质谱全扫描确证火锅料中罂粟壳成分  

Determination of poppy ingredients in chafing dish materials by isotopic internal standard coupled with multiple reaction monitoring and online full scan mass spectrometry

作　　者：祝伟霞 孙转莲 袁萍 杨冀州 刘亚风 孙武勇 

机构地区：[1]河南出入境检验检疫局,河南郑州450003

出　　处：《色谱》2014年第12期1333-1339,共7页Chinese Journal of Chromatography

基　　金：河南省科技攻关项目(122102110167);质检总局科研项目(2007IK162)

摘　　要：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。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（pH3. 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 samples showed this method can be used for the simple and accurate determination of the five poppy alkaloid residues in chafing dish.

关 键 词：高效液相色谱-三重四极杆线性离子阱质谱 增强型子离子全扫描 阳离子固相萃取 生物碱 火锅料 

分 类 号：O658[理学—分析化学]