食品与发酵工业 >

2023 , Vol. 49 >Issue 11: 267 - 272

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.033126

分析与检测

液相色谱-稳定同位素比值质谱测定燕窝中唾液酸的碳稳定同位素比值

  • 冯迪 ,
  • 王道兵 ,
  • 王东亮 ,
  • 钟其顶 ,
  • 武竹英 ,
  • 岳红卫 ,
  • 张洛琪 ,
  • 林小仙 ,
  • 苗树 ,
  • 陈楠楠
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  • 1(国家市场监管技术创新中心(轻工消费品质质量安全,北京,100015))
    2(中国食品发酵工业研究院有限公司,北京,100015)
    3(中轻技术创新中心有限公司,北京,100015)
    4(北京小仙炖生物科技有限公司,北京,100020)
    5(河北省燕窝鲜炖技术创新中心,河北 廊坊,065700)
    6(食品工业推广中心,北京,100015)
硕士研究生(王东亮高级工程师和钟其顶教授级高级工程师为共同通信作者,E-mail:wangdljp@126.com;zhongqingding@163.com)

收稿日期: 2022-07-29

  修回日期: 2022-08-19

  网络出版日期: 2023-06-30

基金资助

北京市朝阳区科技计划项目(CYGX2104);国家重点研发计划项目(2019YFC1605203)

收起

Determination of carbon stable isotope ratios of sialic acid in bird’s nests by liquid chromatography-stable isotope ratio mass spectrometry

  • FENG Di ,
  • WANG Daobing ,
  • WANG Dongliang ,
  • ZHONG Qiding ,
  • WU Zhuying ,
  • YUE Hongwei ,
  • ZHANG Luoqi ,
  • LIN Xiaoxian ,
  • MIAO Shu ,
  • CHEN Nannan
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  • 1(Technology Innovation Center of Light Industrial Consumer Goods Quality and Safety for State Market Regulation, Beijing 100015, China)
    2(China National Research Institute of Food and Fermentation Industries Co.Ltd., Beijing 100015, China)
    3(Sinolight Technology Innovation Centre Co.Ltd., Beijing 100015, China)
    4(Beijing Xiaoxiandun Biotechnology Co.Ltd., Beijing 100020, China)
    5(Hebei Edible Bird’s Nest Fresh Stew Technology Innovation Center, Langfang 065700, China)
    6(Food Industry Promotion Center, Beijing 100015, China)

Received date: 2022-07-29

  Revised date: 2022-08-19

  Online published: 2023-06-30

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摘要

该文建立了适合液相色谱-稳定同位素比值质谱(liquid chromatography-stable isotope ratio mass spectrometry, LC-IRMS)测定干燕窝中唾液酸δ13C值的方法。样品前处理方法加标回收率为75.2%~100.6%,前处理方法可显著降低蛋白质等大分子对色谱柱的影响且不会干扰碳稳定同位素的准确分析;研究并优化了LC-IRMS对唾液酸δ13C值测定的影响,优化后的色谱条件:采用Hyper REZ XP Carbohydrate H+(300 mm×7.7 mm,8 μm)柱,柱温30 ℃,在0.250 mL/min流速下用90% B(H2O)+10% D(pH 2的H2SO4)洗脱。方法稳定性、重复性均良好,可准确测定样品δ13C值。对6个干燕窝样品和4个市售唾液酸进行测定,其唾液酸δ13C值分别为(-29.55±0.39)‰和(-15.18±2.45)‰,2种不同来源唾液酸碳稳定同位素特征显著。可检测到燕窝中的非法掺入市售唾液酸比例最低为10%。该方法的建立可为后续鉴别燕窝制品外源添加唾液酸提供基础。

关键词： 液相色谱-稳定同位素比值质谱; 燕窝; 唾液酸; 前处理; δ13C

本文引用格式

冯迪 , 王道兵 , 王东亮 , 钟其顶 , 武竹英 , 岳红卫 , 张洛琪 , 林小仙 , 苗树 , 陈楠楠 . 液相色谱-稳定同位素比值质谱测定燕窝中唾液酸的碳稳定同位素比值[J]. 食品与发酵工业, 2023 , 49(11) : 267 -272 . DOI: 10.13995/j.cnki.11-1802/ts.033126

Abstract

In this paper, a method was developed for the determination of sialic acid δ13C values in dried bird’s nests by liquid chromatography-stable isotope ratio mass spectrometry (LC-IRMS). The recoveries of the sample off-line pretreatment method ranged from 75.2% to 100.6%, and the pretreatment process could significantly reduce the influence of large molecules such as proteins on the column without causing isotopic fractionation. The effect of LC-IRMS on the determination of δ13C values of sialic acid was investigated and optimized. A Hyper REZ XP Carbohydrate H+ (300 mm×7.7 mm, 8 μm) column with a column temperature of 30 °C was used, eluting with 90% B (H2O) + 10% D (pH 2 H2SO4) at a flow rate of 0.250 mL/min. The method was stable and reproducible for the accurate determination of the δ13C value of sialic acid. Six dried bird’s nest samples and four commercial sialic acids were determined with δ13C values of (-29.55±0.39)‰ and (-15.18±2.45)‰, respectively, and the two different sources of sialic acids had obvious carbon stable isotope characteristics. The percentage of illegally adulterated commercial sialic acid in bird’s nests could be detected at 10%. This method can provide a basis for the subsequent identification of exogenously added sialic acid in bird’s nest products.

Key words： LC-IRMS; bird’s nest; sialic acid; pretreatment; δ13C

参考文献

[1] DAI Y W, CAO J, WANG Y Y, et al.A comprehensive review of edible bird’s nest[J].Food Research International, 2021, 140:109875.
[2] 白伟娟, 林素琼, 柳训才, 等.燕窝真伪鉴别研究进展[J].安徽农学通报, 2020, 26(21):124-127.
BAI W J, LIN S Q, LIU X C, et al.Research progress for authentication of edible bird’s nest[J].Anhui Agricultural Science Bulletin, 2020, 26(21):124-127.
[3] 陈筱婷. 多重RT-PCR法检测燕窝及其制品掺伪成分[J].食品安全质量检测学报, 2019, 10(11):3 493-3 500.
CHEN X T.Determination of adulterated components in edible bird’s nests and their products by multiplex RT-PCR[J].Journal of Food Safety & Quality, 2019, 10(11):3 493-3 500.
[4] 马雪婷, 张九凯, 陈颖, 等.燕窝多元素的分布及溯源信息研究[J].食品与机械, 2019, 35(2):66-71.
MA X T, ZHANG J K, CHEN Y, et al.Study on the distribution characteristics and traceability information of multi-elements in edible bird’s nest[J].Food & Machinery, 2019, 35(2):66-71.
[5] CHUA Y G, CHAN S H, BLOODWORTH B C, et al.Identification of edible bird’s nest with amino acid and monosaccharide analysis[J].Journal of Agricultural and Food Chemistry, 2015, 63(1):279-289.
[6] GUO L L, WU Y J, LIU M C, et al.Determination of edible bird’s nests by FTIR and SDS-PAGE coupled with multivariate analysis[J].Food Control, 2017, 80:259-266.
[7] 岳涛, 王道兵, 李安军, 等.白酒大生产过程中乙醇稳定碳同位素变化特征研究[J].食品与发酵工业, 2023, 49(2):63-67.
YUE T, WANG D B, LI A J, et al.Stable carbon isotopic variation in ethanol during Baijiu processing[J].Food and Fermentation Industries, 2023, 49(2):63-67.
[8] CABAÑERO A I, RECIO J L, RUPÉREZ M.Simultaneous stable carbon isotopic analysis of wine glycerol and ethanol by liquid chromatography coupled to isotope ratio mass spectrometry[J].Journal of Agricultural and Food Chemistry, 2010, 58(2):722-728.
[9] JIN X Y, ZHANG L M, WU S M, et al.Developing an authentication approach using SPME-GC-IRMS based on compound-specific δ13C analysis of six typical volatiles in wine[J].Food Quality and Safety, 2021, 5:31.
[10] 费晓庆, 沈崇钰, 吴斌, 等.元素分析-碳同位素比值质谱法在蜂王浆掺假鉴定中的应用[J].质谱学报, 2014, 35(2):144-148.
FEI X Q, SHEN C Y, WU B, et al.Detection of royal jelly adulteration using elemental analyzer-carbon isotope ratio mass spectrometry[J].Journal of Chinese Mass Spectrometry Society, 2014, 35(2):144-148.
[11] CHOWDHURY S A, CARTER J F, ANUJ S R, et al.The validity of protein in Australian honey as an internal standard for C4 sugar adulteration[J].Food Analytical Methods, 2021, 14(4):823-833.
[12] 钟其顶, 王道兵, 熊正河.稳定氢氧同位素鉴别非还原(NFC)橙汁真实性应用初探[J].饮料工业, 2011, 14(12):6-9.
ZHONG Q D, WANG D B, XIONG Z H.Application of stable hydrogen and oxygen isotope in authenticity assessment of NFC orange juice[J].The Beverage Industry, 2011, 14(12):6-9.
[13] SCHELLENBERG A, CHMIELUS S, SCHLICHT C, et al.Multielement stable isotope ratios (H, C, N, S) of honey from different European regions[J].Food Chemistry, 2010, 121(3):770-777.
[14] ZHANG M J, HU H X, ZENG G F, et al.Discrimination and quantification of adulterated edible bird’s nest based on their improved cohesion stable isotope ratios[J].Food Control, 2022, 140:109111.
[15] PERINI M, BONTEMPO L.Liquid Chromatography coupled to Isotope Ratio Mass Spectrometry (LC-IRMS):A review[J].TrAC Trends in Analytical Chemistry, 2022, 147:116515.
[16] XIONG Q P, HUANG S, CHEN J H, et al.A novel green method for deproteinization of polysaccharide from Cipangopaludina chinensis by freeze-thaw treatment[J].Journal of Cleaner Production, 2017, 142:3 409-3 418.
[17] CHEN L, LONG R, HUANG G L, et al.Extraction and antioxidant activities in vivo of pumpkin polysaccharide[J].Industrial Crops and Products, 2020, 146:112199.
[18] KÖSTER D, SANCHEZ VILLALOBOS I M, JOCHMANN M A, et al.New concepts for the determination of oxidation efficiencies in liquid chromatography-isotope ratio mass spectrometry[J].Analytical Chemistry, 2019, 91(8):5 067-5 073.
[19] DONG H, XIAO K J, XIAN Y P, et al.Authenticity determination of honeys with non-extractable proteins by means of elemental analyzer (EA) and liquid chromatography (LC) coupled to isotope ratio mass spectroscopy (IRMS)[J].Food Chemistry, 2018, 240:717-724.
[20] LEE P L, CLAYTON D H, GRIFFITHS R, et al.Does behavior reflect phylogeny in swiftlets (Aves:Apodidae)? A test using cytochrome b mitochondrial DNA sequences[J].Proceedings of the National Academy of Sciences of the United States of America, 1996, 93(14):7 091-7 096.
[21] CHAN K S, TAN J, GOH W L, et al.Diet profiling of house-farm swiftlets (Aves, Apodidae, Aerodramus sp.) in three landscapes in Perak, Malaysia, using high-throughput sequencing[J].Tropical Ecology, 2019, 60(3):379-388.
[22] CASTILLO-ALANIS L A, GONZÁLEZ-HERNÁNDEZ A E, QUIJANO-MATEOS A, et al.Standardization of a culture medium for Megaselia scalaris (Diptera:Phoridae) for entomotoxicological studies[J].Journal of Medical Entomology, 2020, 57(5):1 421-1 431.
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