SPE-UPLC-MS/MS法同时测定花草茶中的7种吡咯里西啶类生物碱及其氮氧化物  

Simultaneous determination of 7 pyrrolizidine alkaloids and their nitrogen oxides in herbal tea by SPE-UPLC-MS/MS

作　　者：吴钟玲 何仲强 黄志宁 苏锐芬 陈丽婷 钟俊威 WU Zhongling;HE Zhongqiang;HUANG Zhining;SU Ruifen;CHEN Liting;ZHONG Junwei(Collaborative Innovation Center for NQI-Quality Safety of Guangzhou,Guangzhou Quality Supervision and Testing Institute,Guangzhou 511447,China;Guangzhou Institute of Standardization,Guangzhou 510110,China)

机构地区：[1]广州质量监督检测研究院、广州市NQI-质量安全科技协同创新中心,广东广州511447 [2]广州市标准化研究院,广东广州510110

出　　处：《中国酿造》2024年第7期251-256,共6页China Brewing

基　　金：广州市NQI-质量安全科技协同创新中心(2023B04J0407)。

摘　　要：该研究建立了同时测定花草茶中7种吡咯里西啶类生物碱及其氮氧化物(野百合碱、野百合碱-N-氧化物、立可沙明碱、立可沙明碱-N-氧化物、天芥菜碱、天芥菜碱-N-氧化物、千里光宁碱)的固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)分析方法。样品用0.1 mol/L盐酸溶液提取,经MCX固相萃取柱净化后,样液通过Poroshell 120 EC-C_(18)色谱柱(150 mm×3.0 mm,2.7μm)分离,电喷雾正离子多反应监测(MRM)模式检测。结果表明,7种吡咯里西啶类生物碱及其氮氧化物在1.0~50μg/L线性范围呈良好的线性关系,相关系数(R^(2))均>0.998;方法检出限(LOD)和定量限(LOQ)分别为0.3μg/kg和1.0μg/kg。平均加标回收率为81.8%~98.8%,精密度试验结果相对标准偏差(RSD)为1.98%~7.08%。对20个花草茶样品进行检测结果发现,其中有2个样品检出千里光宁碱,分别为18.2μg/kg和33.5μg/kg。该方法快速准确,准确度高,精密度好,适用于花草茶中的吡咯里西啶类生物碱及其氮氧化物的同时测定。A analysis method for simultaneous determination of 7 pyrrolizidine alkaloids and their nitrogen oxides(monocrotaline,monocrotaline N-oxide,lycopsamine,lycopsamine-N-oxide,heliosinine,heliosinine-N-oxide,senecionine)in herbal tea was established by solid phase extraction-ultra high performance liquid chromatography tandem mass spectrometry(SPE-UPLC-MS/MS).The samples were extracted by 0.1 mol/L hydrochloric acid solution and purified by MCX solid phase extraction column,separated by Poroshell 120 EC-C_(18) chromatographic column(150 mm×3.0 mm,2.7μm),and detected by electrospray positive ionization multiple reaction monitoring(MRM)mode.The results showed that the 7 pyrrolizidine alkaloids and their nitrogen oxides showed good linear relationships in the linear range of 1.0-50μg/L,and the correlation coefficients(R^(2))were both greater than 0.998.The limits of detection(LOD)and limits of quantitation(LOQ)were 0.3μg/kg and 1.0μg/kg,respectively.Average spiked recovery rates were 81.8%-98.8%,and the relative standard deviations(RSD)of precision experiment results were 1.98%-7.08%.The results of 20 herbal tea samples tested were found that 2 samples were detected with senecionine,which were 18.2μg/kg and 33.5μg/kg,respectively.The method was rapid,accurate,accurate and suitable for simultaneous determination of pyrrolizidine alkaloids and their nitrogen oxides in herbal tea.

关 键 词：超高效液相色谱-串联质谱法 固相萃取 花草茶 吡咯里西啶类生物碱 氮氧化物 

分 类 号：TS272.5[农业科学—茶叶生产加工] O657.63[轻工技术与工程—农产品加工及贮藏工程]