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
吴钟玲 1何仲强 2黄志宁 1苏锐芬 1陈丽婷 1钟俊威1
作者信息
- 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
- 折叠
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-C18色谱柱(150 mm×3.0 mm,2.7 μm)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1.0～50 μg/L线性范围呈良好的线性关系,相关系数(R2)均＞0.998;方法检出限(LOD)和定量限(LOQ)分别为0.3 μg/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18.2 μg/kg和33.5 μg/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.
Abstract
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-C18 chromatographic column(150 mm×3.0 mm,2.7 μm),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 1.0-50 μg/L,and the correlation coefficients(R2)were both greater than 0.998.The limits of detection(LOD)and limits of quantitation(LOQ)were 0.3 μg/kg and 1.0 μg/kg,respectively.Average spiked recovery rates were 81.8％-9 8.8％,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 18.2 μg/kg and 33.5 μg/kg,respectively.The method was rapid,accurate,ac-curate 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Key words
ultra high liquid chromatography tandem mass spectrometry/solid phase extraction/herbal tea/pyrrolizidine alkaloids/nitrogen oxide引用本文复制引用
基金项目
广州市NQI-质量安全科技协同创新中心(2023B04J0407)
出版年
2024
NETL
NSTL
万方数据