胆碱及其衍生物是一类具有重要生物功能的小分子代谢物，可部分在人体合成，但是更重要的来源是饮食.胆碱被认为是一种人体必需的营养物质，常存在于牛奶、豆类等日常饮食中，也是一种重要的婴儿食品添加剂.饮食中胆碱的长期缺乏与器官功能障碍等疾病有关，因此胆碱衍生物的快速检测分析对食品检测具有重要意义.核磁共振（NMR）技术无需样品分离就可完成相关物质的检测，是理想的食品中胆碱衍生物检测工具.但由于相关分子结构类似，化学位移接近，利用常规NMR技术检测胆碱及其衍生物较为困难.本文采用1H-14N SOFAST-HMQC技术对乳制品中的不同胆碱衍生物进行了快速分析检测，结果发现：与1D 1H NMR谱检测相比，该技术对胆碱衍生物的检测具有高选择性，可消除这些复杂混合体系中其它背景分子干扰；与1H-14N HSQC谱检测技术相比，该技术具有更高的灵敏度，在单位时间内信号增强可达1.5~2.0倍.
柴鑫
,
孙鹏
,
袁斌
,
肖雄杰
,
张许
,
刘买利
. 乳制品中胆碱及其衍生物的快速核磁共振检测[J]. 波谱学杂志, 2018
, 35(2)
: 178
-187
.
DOI: 10.11938/cjmr20172581
Choline containing compounds (CCCs) are a class of small molecule metabolites with important biological functions. Some CCCs can be synthesized by human body, but most of them come from daily diet. CCCs exist in milk, beans, and infant formulas additives. Chronic choline deficiency in the diet is associated with diseases such as organ dysfunction. Therefore, fast detection for CCCs is important for food research. Nuclear magnetic resonance (NMR) spectroscopy is a noninvasive method for CCCs measurement. In this study, 1H-14N SOFAST-HMQC was used to measure the CCCs in dairy products. It was observed that CCCs detection by this method can be more selective than traditional one-dimensional 1H NMR, and the detection sensitivity per unit time was 1.5~2.0 times higher than that of the previous developed 1H-14N HSQC method.
[1] BLUSZTAJN J K. Choline, a vital amine[J]. Science, 1998, 281(5378):794-795.
[2] ILCOL Y O, OZBEK R, HAMURTEKIN E, et al. Choline status in newborns, infants, children, breast-feeding women, breast-fed infants and human breast milk[J]. J Nutr Biochem, 2005, 16(8):489-499.
[3] ARTEGOITIA V M, MIDDLETON J L, HARTE F M, et al. Choline and choline metabolite patterns and associations in blood and milk during lactation in dairy cows[J]. PloS one, 2014, 9(8):103412.
[4] FISCHER L M, DACOSTA K A, KWOCK L, et al. Sex and menopausal status influence human dietary requirements for the nutrient choline[J]. Am J Clin Nutr, 2007, 85(5):1275-1285.
[5] GLUNDE K, BHUJWALLA Z M, RONEN S M. Choline metabolism in malignant transformation[J]. Nat Rev Cancer, 2011, 11(12):835-848.
[6] MAO J Z, JIANG L, JIANG B, et al. A selective NMR method for detecting choline containing compounds in liver tissue:The 1H-14N HSQC experiment[J]. J Am Chem Soc, 2010, 132(49):17349-17351.
[7] MAO X A, LI N, MAO J Z, et al. Fast detection of choline-containing metabolites in liver using 2D 1H-14N three-bond correlation (HN3BC) spectroscopy[J]. J Magn Reson, 2012, 214(1):352-359.
[8] MAO J Z, JIANG L, JIANG B, et al. 1H-14N HSQC detection of choline-containing compounds in solutions[J]. J Magn Reson, 2010, 206(1):157-160.
[9] SCHANDA P, BRUTSCHER B. Very fast two-dimensional NMR spectroscopy for real-time investigation of dynamic events in proteins on the time scale of second[J]. J Am Chem Soc, 2005, 127(22):8014-8015.
[10] SCHANDA P, KUPCE E, BRUTSCHER B. SOFAST-HMQC experiments for recording two-dimensional heteronuclear correlation spectra of proteins within a few seconds[J]. J Biomol NMR, 2005, 33(4):199-211.
[11] SHAKA A J, KEELER J, FREEMAN R. Evaluation of a new broadband decoupling sequence:WALTZ-16[J]. J Magn Reson, 1983, 53(2):313-340.
[12] LIU M L, MAO X A, YE C H, et al. Improved WATERGATE pulse sequences for solvent suppression in NMR spectroscopy[J]. J Magn Reson, 1998, 132(1):125-129.
[13] EMSLEY L, BODENHAUSEN G. Optimization of shaped selective pulses for NMR using a quaternion description of their overall propagators[J]. J Magn Reson, 1992, 97(1):135-148.
[14] MCCOY M A, MUELLER L. Selective shaped pulse decoupling in NMR:homonuclear[carbon-13] carbonyl decoupling[J]. J Am Chem Soc, 1992, 114(6):2108-2112.
[15] GEEN H, FREEMAN R. Band-selective radiofrequency pulses[J]. J Magn Reson, 1991, 93(1):93-141.
[16] KUPCE E, FREEMAN R. Wideband excitation with polychromatic pulses[J]. J Magn Reson, 1994, 108(2):268-273.
[17] ERNST R R, BODENHAUSEN G, VERKOEYEN A著, 毛希安译. 一维和二维核磁共振原理[M]. 北京:科学出版社, 1997.
