中国药物警戒 ›› 2022, Vol. 19 ›› Issue (11): 1186-1190.
DOI: 10.19803/j.1672-8629.20220317

• 基础与临床研究 • 上一篇    下一篇

赤小豆中吡咯里西啶生物碱氮氧化物含量测定及安全风险评估

昝珂1, 周颖2Δ, 李耀磊1, 王莹1, 金红宇1, 左甜甜1#, 马双成1,*   

  1. 1中国食品药品检定研究院,北京 102629;
    2浙江省食品药品检验研究院,国家药品监督管理局中成药质量评价重点实验室,浙江 杭州310052
  • 收稿日期:2022-06-10 发布日期:2022-11-17
  • 通讯作者: *马双成,男,博士,研究员,中药质量控制。E-mail：masc@nifdc.org.cn;#为共同通信作者。
  • 作者简介:昝珂,男,博士,副研究员,中药质量研究。△为并列第一作者。
  • 基金资助:
    国家自然科学基金资助项目（81973476）

Content determination and health risk assessment of pyrrolizidine alkaloid N-oxides in Vignae Semen

ZAN Ke1, ZHOU Ying2Δ, LI Yaolei1, WANG Ying1, JIN Hongyu1, ZUO Tiantian1#, MA Shuangcheng1,*   

  1. 1National Institutes for Food and Drug Control, Beijing 102629, China;
    2Zhejiang Institute for Food and Drug Control, NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Medicine, Traditional Chinese Patent Medicine, Hangzhou Zhejiang 310052, China
  • Received:2022-06-10 Published:2022-11-17

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摘要： 目的 对赤小豆中吡咯里西啶生物碱氮氧化物的含量进行测定和风险评估。方法 采用超高效液相色谱-串联质谱法测定赤小豆中野百合碱氮氧化物、刺凌德草碱氮氧化物、印美定氮氧化物和石松胺氮氧化物的含量。色谱柱采用Acquity UPLC BEH C18（50 mm×2.1 mm, 1.7 μm）,流动相采用乙腈-0.1%甲酸溶液（体积比为10:90）恒流洗脱,流速为0.35 mL·min-1,进样量为2 μL,ESI离子源,正离子MRM模式,以标准曲线法计算含量。根据含量测定结果,采用暴露限值法进行风险评估。结果 8批赤小豆中野百合碱氮氧化物、刺凌德草碱氮氧化物、印美定氮氧化物和石松胺氮氧化物的含量分别为17.54~31.67 μg·kg-1。风险评估显示,使用赤小豆产生的安全风险较低。结论 本研究可为赤小豆中吡咯里西啶生物碱的质量控制和安全性评价提供科学依据。

关键词: 赤小豆, 野百合碱氮氧化物, 刺凌德草碱氮氧化物, 印美定氮氧化物, 石松胺氮氧化物, 超高效液相色谱-串联质谱, 风险评估

Abstract: Objective To determine the contents of pyrrolizidine alkaloid N-oxides in Vignae Semen, and to assess the risks. Methods A UPLC-MS/MS method was established to determine the contents of monocrotaline N-oxide, echinatine N-oxide,intermedine N-oxide and lycosamine N-oxide. An Acquity UPLC BEH C18 (50 mm× 2.1 mm, 1.7 μm) was used as the chromatographic column. The mobile phase was eluted with acetonitrile-0.1% formic acid solution (10:90) at a constant flow rate of 0.35 mL·min-1, and the injection volume was 2 μL. The electrospray spray ion source and positive ion multi-reaction monitoring mode were used. The contents were calculated using the standard curve method. Results The contents of monocrotaline N-oxide, echinatine N-oxide, intermedine N-oxide and lycosamine N-oxide in eight batches of Vignae Semen were 17.54-31.67 μg·kg-1. The risk assessment showed that the health risk of Vignae Semen was low. Conclusion This study provides data for quality control and safety evaluation of pyrrolizidine alkaloids in Vignae Semen.

Key words: Vignae Semen, monocrotaline N-oxide, echinatine N-oxide, intermedine N-oxide, lycosamine N-oxide, UPLC-MS/MS, risk assessment

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