引用本文: | 夏金涛,朱松松,吴婉琴,江丰.基于对照品从头合成策略确证保健食品中非法添加物丙氧基去碳去甲基卡巴地那非[J].中国现代应用药学,2025,42(2):31-30. |
| Xia Jintao,Zhu Songsong,Wu Wanqin,Jiang Feng.Identification of Illegal Additive Propoxydescarbon Desmethyl Carbodenafil in Health Food Based on De Novo Synthesis Strategy of Reference Substance[J].Chin J Mod Appl Pharm(中国现代应用药学),2025,42(2):31-30. |
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摘要: |
目的 采用对照品从头合成策略确证了保健食品中一种新型非法添加卡巴地那非。方法 样品经甲醇提取净化后,进行超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF-MS)非靶向筛查分析,获得分析物的精确分子量和二级碎片离子;经硅胶柱层析分离后,进行核磁共振波谱(NMR)解析,并与从头合成对照品进行比对,最终确定该分析物的结构。 结果 该添加物为丙氧基去碳去甲基卡巴地那非。结论 该分析物未被列入补充检验方法中,作为一种新型添加物首次在保健食品中被检出。 |
关键词: 超高效液相色谱-四极杆-飞行时间质谱 核磁共振波谱 从头合成 保健食品 5型磷酸二酯酶抑制剂(PDE-5) |
DOI: |
分类号:R917;R927.11 |
基金项目:国家市场监督管理总局科技计划项目 |
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Identification of Illegal Additive Propoxydescarbon Desmethyl Carbodenafil in Health Food Based on De Novo Synthesis Strategy of Reference Substance |
Xia Jintao, Zhu Songsong, Wu Wanqin, Jiang Feng
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hubei provincial institute for food supervision and test
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Abstract: |
A new carbodenafil derivative illegally added in health foods was determined by the de novo synthesis strategy of reference substance. METHODS The samples were purified by methanol extraction and injected to ultra-high performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF-MS) for non-targeted screening, the accurate molecular weight and secondary fragment ions of the analyte was then obtained. After separation by silica gel column chromatography, the structure of the analyte was determined by nuclear magnetic resonance spectroscopy (NMR) , and compared with the reference substance from de novo synthesis strategy. RESULTS The additive was propoxydescarbon desmethyl carbodenafil. CONCLUSION The analyte was not included in the additional testing methods and was detected as a novel additive in the dietary supplement for the first time. |
Key words: UPLC-Q-TOF-MS nuclear magnetic resonance spectroscopy de novo synthesis dietary supplement phosphodiesterase type 5 inhibitor (PDE-5) |