基于1H-qNMR的水溶性镧系位移试剂识别法测定功能性食品中谷氨酰胺对映体
作者:
作者单位:

1.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;2.黄冈市中心医院妇产科, 湖北 黄冈 438000

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

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中图分类号:

R155

基金项目:

湖北省自然科学基金青年项目(2021CFB077)


Determination of glutamine enantiomers in functional foods by a water-soluble lanthanide shift reagent-identified method based on the 1H-qNMR technique
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1.Hubei Provincial Institute for Food Supervision and Test, Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-Derived Food for State Market Regulation, Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Hubei Wuhan 430075, China;2.Huanggang Central Hospital, Hubei Huanggang 438000, China

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    摘要:

    目的 建立基于1H-qNMR的水溶性镧系位移试剂识别法,实现对功能性食品中谷氨酰胺(Gln)对映体各自含量的快速定性、定量分析。方法 样品经超纯水溶解,以对苯二甲酸二钠(DT)为内标,经过涡旋、离心后,取适量上层清液于NMR管中,以氘水为锁场溶剂,水溶性镧系位移试剂钐(Ⅲ)-丙二胺四乙酸钠为手性拆分试剂,采用600 MHz核磁共振波谱仪采集1H-NMR谱,直接对功能性食品中的Gln对映体含量进行定量分析。结果 Gln对映体和DT定量峰分离良好。左、右旋Gln的质量浓度在100.0~2 000.0 μg/mL范围内线性良好,R2>0.99,检出限为30.0 μg/mL,定量限为100.0 μg/mL。方法的平均加标回收率为94.27%~116.07%,相对标准偏差(n=6)为0.18%~1.84%。结论 该方法回收率高、重现性好,前处理过程简便,15 min内可完成测样。对商超平台购买的不同剂型功能性食品进行检测,样品中Gln对映体纯度均≥99%。在Gln总量测定方面,该方法与高效液相色谱法检测结果无显著性差异(P>0.05),能够为Gln对映体含量的快速检测提供一种实用的技术。

    Abstract:

    Objective This study aimed to achieve rapid qualitative and quantitative analysis of the respective contents of glutamine (Gln) enantiomers in functional foods by establishing a water-soluble lanthanide shift reagent-identified method based on the 1H-qNMR technique.Methods The internal standard disodium terephthalate was added to the samples dissolved in ultrapure water. After vertexing and centrifuging, an appropriate amount of supernatant was taken into the NMR tube with deuterium water as a field-locking solvent and the water-soluble lanthanide shift reagent samarium (Ⅲ)-propylenediaminetetraacetate as the chiral selector. The 1H-NMR spectrum was collected by a 600 MHz nuclear magnetic resonance spectrometer for the direct determination of the contents of Gln enantiomers in functional foods.Results The Gln enantiomers and DT quantitative peaks were well-separated. The mass concentration of D- and L-glutamine has a good linearity in the range of 100.0-2 000.0 μg/mL with R2>0.99. The limit of detection was 30.0 μg/mL, and the limit of quantification was 100.0 μg/mL. The average recovery rates obtained from standard addition methods were between 94.27% and 116.07% with the relative standard deviations (n=6) being 0.18%-1.84%.Conclusion This method offers high recovery, good repeatability, and a simple pretreatment process, and the sample test can be completed within 15 min. The testing of different dosage forms of functional foods purchased from the supermarket platform revealed that the enantiomeric purity of Gln in the samples was ≥99%. No significant difference was observed between this method and high-performance liquid chromatography (P>0.05) in the determination of total Gln. The method can provide a practical technique for the rapid detection of the contents of glutamine enantiomers.

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夏金涛,黄秀秀,朱松松,朱芊,李贝贝,江丰.基于1H-qNMR的水溶性镧系位移试剂识别法测定功能性食品中谷氨酰胺对映体[J].中国食品卫生杂志,2023,35(11):1579-1586.

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  • 收稿日期:2022-07-11
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