成分分析

QuEChERS-UPLC-MS/MS法快速测定蜂蜜中28个吡咯里西啶生物碱的含量及风险评估*

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  • 中国食品药品检定研究院,北京 102629
第一作者 Tel:(010)53852092; E-mail:6206310@qq.com
**马双成 Tel:(010)53852076; E-mail:masc@nifdc.org.cn
左甜甜 Tel:(010)53851453; E-mail:zuotiantian2011@163.com

收稿日期: 2021-04-27

  网络出版日期: 2024-06-25

基金资助

*科技部重大新药创制 (项目编号:2018ZX09303-024,2018ZX09735-006)

Risk assessment and fast determination of 28 pyrrolizidine alkaloids in honey by QuEChERS method and UPLC-MS/MS*

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  • National Institutes for Food and Drug Control, Beijing 102629, China

Received date: 2021-04-27

  Online published: 2024-06-25

摘要

目的:建立基于QuEChERS结合超高效液相色谱-串联质谱(UPLC-MS/MS)测定蜂蜜中28个吡咯里西啶生物碱的快速检测方法,并根据测定结果进行初步的风险评估。方法:采用QuEChERS法对样品进行前处理,ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm, 1.8 μm),以含0.05%甲酸和2.5 mmol·L-1甲酸铵的水溶液(A)及含0.05%甲酸和2.5 mmol·L-1甲酸铵的乙腈溶液(B)为流动相,梯度洗脱,流速为0.3 mL·min-1,柱温为40 ℃;电喷雾离子源为正离子多反应监测模式,外标法测定。结果:28个吡咯里西啶生物碱在1~20 ng·mL-1内线性关系良好,相关系数均大于0.99;平均回收率为71.8%~103.5%,RSD为3.3%~9.2%。28个吡咯里西啶生物碱的定量下限为0.20~0.90 ng·mL-1;30批样品中有10批样品检出吡咯里西啶生物碱,阳性样品中总含量为4.85~78.34 μg·kg-1结论:该方法操作简便快速、准确、灵敏,可同时测定蜂蜜中28个吡咯里西啶生物碱含量。初步风险评估显示,蜂蜜存在一定的安全风险。

本文引用格式

昝珂, 李耀磊, 王莹, 刘丽娜, 金红宇, 左甜甜, 马双成 . QuEChERS-UPLC-MS/MS法快速测定蜂蜜中28个吡咯里西啶生物碱的含量及风险评估*[J]. 药物分析杂志, 2021 , 41(12) : 2087 -2094 . DOI: 10.16155/j.0254-1793.2021.12.06

Abstract

Objective: To establish a method for the simultaneous determination of 28 pyrrolizidine alkaloids in honey by QuEChERS and UPLC-MS/MS, and carry out preliminary risk assessment according to the research results. Methods: The samples were prepared by QuEChERS, then separated on an ACQUITY UPLC HSS T3 column (2.1 mm×100 mm, 1.8 μm). The sample was eluted with a gradient mobile phase consisting of 0.05% formic acid and 2.5 mmol·L-1 ammonium formate in water(A)-0.05% formic acid and 2.5 mmol·L-1 ammonium formate in acetonitrile(B). The flow rate was 0.3 mL·min-1 and the column temperature was 40 ℃. The MS system was operated by using electrospray ionization (ESI) in the positive ion mode, and the scan mode was in multiple reactions monitoring (MRM) mode. External standard method was used in the experiment. Results: The results showed that all the 28 PAs had good linearity in 1-20 ng·mL-1 with the correlation coefficients higher than 0.99. The average recoveries of all the 28 PAs were between 71.8% and 103.5%, with the RSDs of 3.3%-9.2%. The limits of quantifications (LOQs) of 28 PAs were between 0.20 ng·mL-1 and 0.90 ng·mL-1. PAs was detected in 10 of 30 samples, and the total contents of positive samples were 4.85-78.34 μg·kg-1. Conclusion: The established method can simultaneously determine 28 pyrrolizidine alkaloids in honey. The preliminary risk assessment shows that there is a certain risk of drug safety.

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