高效液相色谱法测定鸡蛋、鸡肉中五种类胡萝卜素物质

兰韬 闫娜 裴栋 刘佳雯 于聪聪 初侨 李笃信

兰韬,闫娜,裴栋,等. 高效液相色谱法测定鸡蛋、鸡肉中五种类胡萝卜素物质[J]. 食品工业科技,2021,42(20):261−267. doi:  10.13386/j.issn1002-0306.2021010109
引用本文: 兰韬,闫娜,裴栋,等. 高效液相色谱法测定鸡蛋、鸡肉中五种类胡萝卜素物质[J]. 食品工业科技,2021,42(20):261−267. doi:  10.13386/j.issn1002-0306.2021010109
LAN Tao, YAN Na, PEI Dong, et al. Determination of Five Carotenoids in Eggs and Chicken by HPLC[J]. Science and Technology of Food Industry, 2021, 42(20): 261−267. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2021010109
Citation: LAN Tao, YAN Na, PEI Dong, et al. Determination of Five Carotenoids in Eggs and Chicken by HPLC[J]. Science and Technology of Food Industry, 2021, 42(20): 261−267. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2021010109

高效液相色谱法测定鸡蛋、鸡肉中五种类胡萝卜素物质

doi: 10.13386/j.issn1002-0306.2021010109
基金项目: 国家市场监督管理总局技术保障专项项目(2020YJ044);青岛市科技惠民示范引导专项(20-3-4-11-nsh)
详细信息
    作者简介:

    兰韬(1984−),男,博士,副研究员,研究方向:农产品标准样品,E-mail:lantao@cnis.ac.cn

    通讯作者:

    李笃信(1982−),男,博士,副教授,研究方向:分析化学,E-mail:douglas086@qq.com

  • 中图分类号: TS253.7

Determination of Five Carotenoids in Eggs and Chicken by HPLC

  • 摘要: 本文研究了鸡蛋、鸡肉中虾青素、叶黄素、斑蝥黄、玉米黄素、β-胡萝卜素等5种类胡萝卜素同时检测的HPLC方法。结果表明,5种类胡萝卜素在0.5~100 μg/mL线性范围内有较好的线性关系,决定系数R2均大于0.996,方法的检出限均在0.10~0.20 mg/kg之间,定量限在0.33~0.66 mg/kg之间。在1、10、20 mg/kg的加标水平下,鸡蛋和鸡肉样品的加标回收率分别在71.6%~112.9%和88.6%~119.7%之间,RSD均≤7.2%。该方法快速简单、准确度高、重复性好,适用于鸡蛋、鸡肉等复杂基质样品中5种类胡萝卜素类物质检测的要求,对于鸡蛋、鸡肉的市场监管具有重要意义。
  • 图  1  三种流动相体系下5种类胡萝卜素的色谱分离图

    Figure  1.  Chromatogram of 5 carotenes under three mobile phase systems

    注:(a):乙腈−0.1%甲酸水溶液;(b):乙腈-氯仿;(c):乙腈-二氯甲烷;1:虾青素;2:叶黄素;3:玉米黄素;4:斑蝥黄;5:β-胡萝卜素。

    表  1  2种不同溶剂提取结果对比

    Table  1.   Comparison of extraction results of two different solvent

    来源分析物乙腈提取,正己烷脱脂 60%二氯甲烷/乙腈提取
    回收率(%)RSD(%)回收率(%)RSD(%)
    鸡蛋虾青素89.10.9105.00.4
    叶黄素74.20.789.70.5
    玉米黄素67.20.589.21.1
    斑蝥黄85.87.396.60.2
    β-胡萝卜素24.64.4110.52.1
    鸡肉虾青素38.26.6110.80.9
    叶黄素69.54.1108.91.1
    玉米黄素60.84.497.66.1
    斑蝥黄51.10.6115.61.0
    β-胡萝卜素9.52.5113.00.9
    下载: 导出CSV

    表  2  5种类胡萝卜素物质的线性范围、LOD和LOQ

    Table  2.   Linear range, LOD and LOQ of 5 carotenes

    组分线性范围(μg/mL)线性方程R2LOD(mg/kg)LOQ(mg/kg)
    虾青素0.5~100Y=140.8X−92.00.99950.100.33
    叶黄素0.5~100Y=46.2X−78.70.99680.200.66
    玉米黄素0.5~100Y=25.9X−56.50.99790.200.66
    斑蝥黄0.5~100Y=105.0X−64.60.99980.100.33
    β-胡萝卜素0.5~100Y=106.6X−260.20.99730.100.33
    下载: 导出CSV

    表  3  方法的重复性试验结果(n=6)

    Table  3.   Repeatability test results of this method(n=6)

    组分鸡肉样品重复性RSDs(%)鸡蛋样品重复性RSDs(%)
    虾青素4.53.3
    叶黄素3.12.0
    玉米黄素3.23.9
    斑蝥黄2.34.8
    β-胡萝卜素1.92.6
    下载: 导出CSV

    表  4  鸡蛋、鸡肉样品的加标回收试验结果

    Table  4.   Recoveries of 5 carotenes in egg and chicken samples

    组分加标水平(1 mg/kg) 加标水平(10 mg/kg) 加标水平(20 mg/kg)
    回收率RSDs(%)回收率RSDs(%)回收率RSDs(%)
    鸡蛋虾青素105.51.0110.06.2105.00.4
    叶黄素95.82.498.12.489.70.5
    玉米黄素90.22.771.65.489.21.1
    斑蝥黄101.01.385.96.696.60.2
    β-胡萝卜素112.92.1108.26.9110.52.1
    鸡肉虾青素118.15.8111.01.5110.80.9
    叶黄素111.95.7100.91.8108.91.1
    玉米黄素119.72.1110.53.897.66.1
    斑蝥黄116.36.9115.91.6115.61.0
    β-胡萝卜素88.67.2107.24.9113.00.9
    下载: 导出CSV

    表  5  鸡蛋、鸡肉样品的基质效应

    Table  5.   Matrix effect of egg and chicken samples

    组分标准溶液的线性方程(A)基质溶液的线性方程(B)斜率比B/A
    鸡蛋虾青素Y=123.9X−8.7Y=123.6X−15.20.998
    叶黄素Y=41.5X−69.5Y=40.6X−29.20.978
    玉米黄素Y=18.2X−120.6Y=18.8X−37.11.032
    斑蝥黄Y=144.0X−10.6Y=145.1X−2.41.008
    β-胡萝卜素Y=84.5X−470.2Y=93.1X+13.01.101
    鸡肉虾青素Y=121.7X−37.9Y=109.6X−16.70.900
    叶黄素Y=43.7X−135.5Y=45.9X−5.61.051
    玉米黄素Y=19.4X−83.3y=19.4X−83.31.000
    斑蝥黄Y=84.3X−15.1Y=76.9X−13.90.912
    β-胡萝卜素Y=111.9X−999.2Y=102.2X−12.90.914
    下载: 导出CSV

    表  6  不同鸡蛋鸡肉样品中5种类胡萝卜素含量

    Table  6.   Contents of 5 carotenes in egg and chicken samples

    样品虾青素(mg/g)叶黄素(mg/kg)玉米黄素(mg/kg)斑蝥黄(mg/kg)β-胡萝卜素(mg/kg)
    鸡蛋11.31.75.60.31.5
    鸡蛋22.66.92.5未检出0.8
    鸡肉10.41.11.4未检出1.8
    鸡肉20.20.80.91.22.9
    下载: 导出CSV
  • [1] 李红霞, 徐聪, 杨兰兰, 等. 加丽素红在动物性食品中安全性的研究进展[J]. 云南畜牧兽医,2015(2):23−25. [Li H X, Xu C, Yang L L, et al. Research progress on the safety of garlicol red in animal food[J]. Yunnan Animal Husbandry and Veterinary,2015(2):23−25. doi:  10.3969/j.issn.1005-1341.2015.02.017
    [2] 李俊, 程业飞, 苏越, 等. 阿朴酯和斑螯黄复合对蛋鸡抗氧化功能、蛋品质和蛋黄色素沉积的影响[J]. 湖北农业科学,2018,57(18):88−91. [Li J, Cheng Y F, Su Y, et al. Effects of aposter combined with canthaxanthin on antioxidant function, egg quality and yolk pigment deposition in laying hens[J]. Hubei Agricultural Sciences,2018,57(18):88−91.
    [3] Dias M G, Camo˜es M F, Oliveira L. Measurement uncertainty of food carotenoid determination[J]. Accreditation and Quality Assurance,2012,17:183−189. doi:  10.1007/s00769-011-0870-2
    [4] 李福枝, 刘飞, 曾晓希, 等. 天然类胡萝卜素的研究进展[J]. 食品工业科技,2007,28(9):227−232. [Li F Z, Liu F, Zeng X X, et al. The research progress of natural carotenoid[J]. Science and Technology of Food Industry,2007,28(9):227−232. doi:  10.3969/j.issn.1002-0306.2007.09.069
    [5] 付淑梅, 刘婷. 反相高效液相色谱法测定饲料中的斑蝥黄含量[J]. 广东化工,2017,44(16):233−234. [Fu S M, Liu T. Analysis of canthaxanthin content in feed by RP-HPLC[J]. Guangdong Chemical Industry,2017,44(16):233−234. doi:  10.3969/j.issn.1007-1865.2017.16.107
    [6] 刘艳芳. 土鸡蛋中类胡萝卜素的提取、分离鉴定及其稳定性研究[D]. 武汉: 华中农业大学, 2010.

    Liu Y F. Extraction, isolation, identification and stability of carotenoids from native eggs[D]. Wuhan: Huazhong Agricultural University, 2010.
    [7] 宗万里, 臧汝瑛, 宋韶锦. 液相色谱-四级杆/静电场轨道阱高分辨质谱测定鸡蛋中斑蝥黄含量[J]. 黄河科技学院学报,2019,21(5):94−97. [Zong W L, Zang R Y, Song S J. Determination of canthaxanthin in eggs by liquid chromatography-quadrupole/electrostatic field orbital trap high resolution mass spectrometry[J]. Journal of Huanghe S & T College,2019,21(5):94−97.
    [8] 张彩凌, 牛春芳, 葛兴信, 等. 高效液相色谱法测定栅藻中5种类胡萝卜素的含量[J]. 分析科学学报,2016,32(2):269−272. [Zhang C L, Niu C F, Ge X X, et al. Determination of five carotenes in scendesmus by high performance liquidchromatography[J]. Journal of Analytical Science,2016,32(2):269−272.
    [9] Jia J, Wang Y, Liu Y, et al. Exploration of interaction of canthaxanthin with human serum albumin by spectroscopic and molecular simulation methods[J]. Luminescence,2018,33:425−432. doi:  10.1002/bio.3430
    [10] Animal feed-brighter eyesight or brighter salmon? Commission decides new rules on colouring feed additive[EB/OL]. (2002-01-27)[2013-09-03]. http://www.foodlaw.rdg.ac.uk/news/eu-03009.html.
    [11] Evaluations of the joint FAO/WHO expert committee on food additives(JECFA) canthaxanthin[EB/OL]. http://apps.Who.int/food-additives-contaminants-jecfa-database/chemical.aspx?chemID=1268.
    [12] The Japan Food Chemical Research Foundation. Maximum residue limits(MRLs) list of agricultural chemicals in foods[EB/OL]. [2015-11-20]. http://db.ffcr.or.jp/front/.
    [13] 《饲料添加剂安全使用规范》(2017年修订版)(农业农村部公告第2625号)[EB/OL]. http://www.moa.gov.cn/nybgb/2018/201801/201801/t20180129_6135954.htm

    Code for safe use of feed additives (revised in 2017) (Announcement No. 2625 of the ministry of agriculture and rural areas) [EB/OL]. http://www.moa.gov.cn/nybgb/2018/201801/201801/t20180129_6135954.htm
    [14] 赵婷, 惠伯棣, 裴凌鹏. 斑蝥黄质在雄性大鼠血清中的积累研究[J]. 食品科学,2012,33(5):260−262. [Zhao T, Hui B D, Pei L P. A preliminary investigation into canthaxanthin accumulation in male rat serum[J]. Food Science,2012,33(5):260−262.
    [15] 郑国建, 关岩, 杨方, 等. 高效液相色谱法检测婴幼儿奶粉中的叶黄素[J]. 中国乳品工业,2016,44(1):51−53. [Zheng G J, Guan Y, Yang F, et al. Lutein determination by HPLC in infant formula[J]. China Dairy Industry,2016,44(1):51−53. doi:  10.3969/j.issn.1001-2230.2016.01.012
    [16] Ligor M, Kováčová J, Gadzała-Kopciuch R M, et al. Study of RP HPLC retention behaviours in analysis of carotenoids[J]. Chromatographia,2014,77(15−16):1047−1057. doi:  10.1007/s10337-014-2657-1
    [17] Aman R, Bayha S, Carle R, et al. Determination of carotenoid stereoisomers in commercialdietary supplements by high-performance liquid chromatography[J]. Journal of Agricultural and Food Chemistry,2004,52:6086−6090. doi:  10.1021/jf049304l
    [18] Brizio P, Benedetto A, Righetti M, et al. Astaxanthin and canthaxanthin(xanthophyll) as supplements in rainbow trout diet: In vivo assessment of residual levels and contributions to human health[J]. Journal of Agricultural & Food Chemistry,2013,61(46):10954−10959.
    [19] 焦广睿, 王柯. 高效液相色谱-串联质谱法测定蛋黄中4种类胡萝卜素着色剂的含量[J]. 上海预防医学,2018,30(6):472−475. [Jiao G R, Wang K. Simultaneous determination of 4 carotenoid pigments in yolk by liquid chromatography-tandem mass spectrometry[J]. Shanghai Journal of Preventive Medicine,2018,30(6):472−475.
    [20] Bergantin C, Maietti A, Tedeschi P, et al. HPLC-UV/Vis-APCI-MS/MS determination of major carotenoids and their bioaccessibility from “Delica”(Cucurbita maxima) and “Violina”(Cucurbita moschata) pumpkins as food traceability markers[J]. Molecules,2018,23:2791. doi:  10.3390/molecules23112791
    [21] 惠伯棣, 李京, 孙拿拿, 等. 番茄和胡萝卜中类胡萝卜素的C30与C18HPLC分离[J]. 中国食品卫生杂志,2006,18(4):289−292. [Hui B D, Li J, Sun N N, et al. C30 and C18 HPLC separation of carotenoids from plant foods[J]. Chinese Journal of Food Hygiene,2006,18(4):289−292. doi:  10.3969/j.issn.1004-8456.2006.04.001
    [22] 国家标准委农业食品部. GB/T 22958-2008 河豚鱼、鳗鱼和烤鳗中角黄素残留量的测定液相色谱-紫外检测法[S]. 北京: 中国标准出版社, 2008.

    Ministry of Agriculture and Food, National Standards Commission. GB/T 22958-2008 Determination of canthaxanthin residues in fugu, eel and baked eel-HPLC-UV method[S]. Beijing: China Standards Press, 2008.
    [23] 农业农村部. NY/T 2896-2016 饲料中斑蝥黄的测定高效液相色谱法[S]. 北京: 中国标准出版社, 2016.

    Ministry of Agri-culture and Rural Areas. NY/T 2896-2016 Determination of canthaxanthin in feeds-high performance liquid chromatography[S]. Beijing: China Standards Press, 2016.
    [24] Furusawa N. A simple and small-scale sample preparation technique to determine canthaxanthin in hen egg yolk[J]. Food Chemistry,2011,124(4):1643−1646. doi:  10.1016/j.foodchem.2010.08.017
    [25] 陈东洋, 张昊, 冯家力, 等. 固相萃取-高效液相色谱法测定禽蛋中斑蝥黄和叶黄素[J]. 中国食品卫生杂志,2020,32(1):45−49. [Chen D Y, Zhang H, Feng J L, et al. Determination of canthaxanthin and xanthophyll in eggs by SPE-high performance liquid chromatography[J]. Chinese Journal of Food Hygiene,2020,32(1):45−49.
    [26] 白杰, 屈殷子, 王珊珊, 等. 限域结晶法制备载β-胡萝卜素的氧化淀粉水凝胶球[J]. 食品科学,2020,41(8):1−7. [Bai J, Qu Y, Wang S, et al. Preparation of oxidized starch hydrogel encapsulating β-carotene by confined crystallization[J]. Food Science,2020,41(8):1−7. doi:  10.7506/spkx1002-6630-20190103-043
    [27] 余孔捷, 钱疆, 杨方, 等. 高效液相色谱法测定动物源性食品中角黄素、虾青素的研究[J]. 食品与发酵工业,2008,34(3):145−148. [Yu K, Qian J, Yang F, et al. Determination of canthaxanthin and astaxanthin in animal origin food by HPLC[J]. Food and Fermentation Industries,2008,34(3):145−148.
    [28] 郝东宇, 席兴军, 初侨, 等. 快速滤过型净化法结合高效液相色谱-串联质谱 同时检测人参中的5种农药残留[J]. 农药学学报,2019,21(1):82−88. [Hao D, Xi X, Chu Q, et al. Simultaneous detection of five pesticide residues in ginseng by multi-plug filtration cleanup method combined with high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science,2019,21(1):82−88.
    [29] Yu C C, Hao D Y, Chu Q, et al. A one adsorbent QuEChERS method coupled with LC-MS/MS forsimultaneous determination of 10 organophosphorus pesticide residues intea[J]. Food Chemistry,2020,321:126657. doi:  10.1016/j.foodchem.2020.126657
    [30] 马立利, 贾丽, 周欣燃, 等. 多壁碳纳米管滤过型净化柱净化-超高效液相色谱串联质谱法同时测定生姜中的涕灭威及其代谢物[J]. 色谱,2014,32(6):635−639. [Ma L L, Jia L, Zhou X R, et al. Analysis of aldicarb and its metbbolites in ginger using ultra performance liquid chromatograghy-tandem mass spectrometry coupled with multiplug filtration clean up with multiwalled carbon nanotubes[J]. Chinese Journal of Chromatography,2014,32(6):635−639. doi:  10.3969/j.issn.1000-8713.2014.06.013
    [31] 兰韬, 初侨, 郝东宇, 等. Sin-QuEChERS结合UPLC-MS/MS同时检测茶叶中10种有机磷农药残留[J]. 质谱学报,2019,40(3):268−279. [Lan T, Chu Q, Hao D, et al. Simultaneously detection of 10 organophosphorus pesticides residues in tea by Sin-QuEChERS with UPLC-MS/MS[J]. Journal of Chinese Mass Spectrometry Society,2019,40(3):268−279. doi:  10.7538/zpxb.2018.0123
  • 加载中
图(1) / 表(6)
计量
  • 文章访问数:  67
  • HTML全文浏览量:  29
  • PDF下载量:  15
  • 被引次数: 0
出版历程
  • 收稿日期:  2021-01-15
  • 网络出版日期:  2021-08-04
  • 刊出日期:  2021-10-11

目录

    /

    返回文章
    返回

    重要通知

    喜报:《食品工业科技》2021版影响因子稳居第二,且影响因子大幅提升