手性镧系位移试剂识别-核磁共振氢谱法测定保健食品中肉碱对映体含量
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作者单位:

湖北省食品质量安全监督检验研究院,国家市场监管重点实验室 动物源性食品中重点化学危害物 检测技术 湖北省食品质量安全检测工程技术研究中心,湖北 武汉 430075

作者简介:

夏金涛 男 工程师 研究方向为食品安全与检测 E-mail: 2501820896@qq.com

通讯作者:

江丰 男 高级工程师 研究方向为食品安全与检测 E-mail: 349136833@qq.com

中图分类号:

R155

基金项目:

湖北省自然科学基金青年项目(2021CFB077);国家重点研发计划项目(2018YFC1602300)


Determination of carnitine enantiomers in dietary supplement by 1H-nuclear magnetic resonance combined with chiral lanthanide shift reagents
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Affiliation:

Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-derived Food for State Market Regulation, Hubei Provincial Institute for Food Supervision and Test, Hubei Wuhan 430075, China

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    摘要:

    目的 采用手性镧系位移试剂识别-核磁共振氢谱法(CLSR-1H qNMR)对保健食品中的肉碱对映体进行快速定性、定量分析研究。方法 样品经氘代甲醇溶解,以吡嗪为内标,经过涡旋、超声辅助萃取、离心后,取适量上层清液,加入手性镧系位移试剂Eu(thfc)3,直接对待测物进行检测。结果 左旋肉碱的质量浓度线性范围在16.3~4 800 μg/mL,相关系数(r)>0.99,检出限(LOD)为24.5 mg/kg,定量限(LOQ)为73.5 mg/kg;右旋肉碱的质量浓度线性范围在10.6~530 μg/mL,r>0.99,LOD为27.5 mg/kg,LOQ为82.5 mg/kg。方法的加标回收率为95.9%~114.6%,RSD(n=6)为3.31%~6.12%。对网购宣称具有减肥功效的胶囊、奶茶、咖啡粉、片剂进行检测,均未检测出右旋肉碱。结论 本方法简便、快速、灵敏,25 min内即可完成检测,能够为肉碱对映体各自含量的快速检测提供理论基础。

    Abstract:

    Objective A qualitative and quantitative method has been established to rapidly determine carnitine enantiomers in dietary supplement by 1H-nuclear magnetic resonance combined with chiral lanthanide shift reagents (CLSR-1H qNMR).Methods Pyrazine acted as internal standard was added to the samples dissolved in d4-methanol. After vortexing, ultrasonic-assisted extraction and centrifugation, an appropriate amount of supernatant and chiral lanthanide shift reagent (CLSR) Eu(thfc)3 were added to the NMR tube for directly determination.Results The linearity range of L-carnitine was 16.3~4 800 μg/mL with correlation coefficient (r)>0.99. The limit of detection (LOD) was 24.5 mg/kg, and the limit of quantification (LOQ) was 73.5 mg/kg. While the linearity range of D-carnitine was 10.6~530 μg/mL with r>0.99. The LOD was 27.5 mg/kg, and the LOQ was 82.5 mg/kg. Recovery rates obtained from spiked samples were between 95.9% and 114.6% with the RSDs (n=6) of 3.31%~6.12%. Tests on capsules, milk tea, coffee powder and tablet from online shopping that claimed to have weight-loss effects failed to detect D-carnitine.Conclusion This method is simple, rapid and sensitive. And the sample test could be completed within 25 min, which could provide a theoretical basis for rapidly detection of carnitine enantiomers.

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夏金涛,朱松松,朱芊,江丰.手性镧系位移试剂识别-核磁共振氢谱法测定保健食品中肉碱对映体含量[J].中国食品卫生杂志,2022,34(4):730-736.

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  • 收稿日期:2022-02-17
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  • 在线发布日期: 2022-08-26
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