LI Shuo, LI Li. Determination of Nodularin in Algae-based Health Food by Ultra- Performance Liquid Triple Quadrupole Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2022, 43(6): 287−292. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021070020.
Citation: LI Shuo, LI Li. Determination of Nodularin in Algae-based Health Food by Ultra- Performance Liquid Triple Quadrupole Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2022, 43(6): 287−292. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021070020.

Determination of Nodularin in Algae-based Health Food by Ultra- Performance Liquid Triple Quadrupole Chromatography-Tandem Mass Spectrometry

More Information
  • Received Date: July 01, 2021
  • Available Online: January 14, 2022
  • A method was developed for the determination of nodularin (NOD) in algae-based health food by ultra-performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-MS/MS). The analytes were extracted from algae-based health food powder with methanol/water (80:20, v/v), and purified before analysis. The separation of analytes was performed on an Agilent Infinity Poroshell 120 SB-C18 chromatographic column (2.1 mm×100 mm, 2.7 μm) with the gradient elution of acetonitrile and water (containing 0.01% formic acid) as mobile phases. Qualitative analysis was performed by multiple reaction monitoring (MRM) mode. Matrix matched standard curve was used for quantitative analysis. The chromatographic and MS parameters were optimized. Major factors affecting the extraction and clean-up efficiencies including the type of extraction solvent and clean-up cartridges were investigated. The nodularin had a good linear relationship in range of 0.5~50 μg/L and correlation coefficient (r) was 0.9997. The limit of detection (LOD, S/N=3) and limit of quantification (LOQ, S/N=10) were 1 and 3 μg/kg, respectively. The spiked recoveries of nodularin at 3 spiked levels were 103.6%~114.8%, and relative standard deviations (RSD) were 3.3%~12.5% (n=6). The established method was simple, rapid and quantitatively accurate, which was suitable for quick analysis of nodularin in algae-based health food.
  • [1]
    江敏, 许慧. 节球藻毒素研究进展[J]. 生态学报,2014,34(16):4473−4479. [JIANG M, XU H. Research progress of nodularin[J]. Acta Ecologica Sinica,2014,34(16):4473−4479.
    [2]
    朱小奕, 陈瑾, 张建英. 水环境中藻毒素生态风险的物种敏感性分布评价[J]. 生态毒理学报,2016,11(3):131−139. [ZHU X Y, CHEN J, ZHANG J Y. Assessing ecological risk of cyanotoxins based on interspecies correlation estimation and species sensitivity distributions[J]. Asian Journal of Ecotoxicology,2016,11(3):131−139.
    [3]
    郝纪蓉, 李云团, 江敏, 等. 节球藻毒素对斑马鱼胚胎发育的毒性效应[J]. 生态毒理学报,2013,8(4):587−594. [HAO J R, LI Y T, JIANG M, et al. Toxic effects of nodularin on zebrafish (Danio rerio) embryo[J]. Asian Journal of Ecotoxicology,2013,8(4):587−594. doi: 10.7524/AJE.1673-5897.20121110002
    [4]
    CANEDO A, ROCHA T L. Zebrafish (Danio rerio) using as model for genotoxicity and DNA repair assessments: Historical review, current status and trends[J]. Science of the Total Environment,2021,762:144084. doi: 10.1016/j.scitotenv.2020.144084
    [5]
    AMBER B, AMANDA F, MELISSA A M, et al. Detection of cyanotoxins (microcystins/nodularins) in livers from estuarine and coastal bottlenose dolphins (Tursiops truncatus) from Northeast Florida[J]. Harmful Algae,2018,76:22−34. doi: 10.1016/j.hal.2018.04.011
    [6]
    CHEN G L, WANG L P, WANG M X, et al. Comprehensive insights into the occurrence and toxicological issues of nodularins[J]. Marine Pollution Bulletin,2021,162:111884. doi: 10.1016/j.marpolbul.2020.111884
    [7]
    International Agency for Research on Cancer. List of classifications [DB/OL] (2021-07-22)[2021-09-17]. https://monographs.iarc.who.int/list-of-classifications.
    [8]
    王志钢, 刘彬, 于春媛, 等. 藻类保健功能及保健食品应用与开发[J]. 中国食物与营养,2020,26(12):27−30. [WANG Z G, LIU B, YU C Y, et al. Health function of algae and the development of health foods[J]. Food and Nutrition in China,2020,26(12):27−30. doi: 10.3969/j.issn.1006-9577.2020.12.007
    [9]
    杜鹏, 张晓娜, 董诗源. 藻类保健食品研发状况及问题探讨[J]. 海峡预防医学杂志,2020,26(6):73−75. [DU P, ZHANG X N, DONG S Y. Research and development status of algae health food and the existing problems[J]. Strait Journal of Preventive Medicine,2020,26(6):73−75.
    [10]
    徐海滨, 陈艳, 李芳, 等. 螺旋藻类保健食品生产原料及产品中微囊藻毒素污染现状调查[J]. 卫生研究,2003,32(4):339−343. [XU H B, CHEN Y, LI F, et al. Investigation of concentration of microcystin in raw materials and finished products of spires health food[J]. Journal of Hygiene Research,2003,32(4):339−343. doi: 10.3969/j.issn.1000-8020.2003.04.008
    [11]
    欧阳生群, 胡波, 周蓉, 等. 基于HT-SELEX筛选的节球藻毒素-R适配体的鉴定[J]. 中国生物化学与分子生物学报,2018,34(1):69−76. [OUYANG S Q, HU B, ZHOU R, et al. The characterization of nodularin-R specific aptamer obtained from HT-SELEX[J]. Chinese Journal of Biochemistry and Molecular Biology,2018,34(1):69−76.
    [12]
    王婧, 江敏, 许慧, 等. 节球藻毒素的紫外光降解研究[J]. 环境科学学报,2016,36(7):2517−2524. [WANG J, JIANG M, XU H, et al. Degradation of nodularin by ultraviolet light(UV)[J]. Acta Scientiae Circumstantiae,2016,36(7):2517−2524.
    [13]
    国家技术监督局. GB/T 16919-1997使用螺旋藻粉[S]. 北京: 中国标准出版社, 1997.

    State Bureau of Technical Supervision. GB/T 16919-1997 Food grade spirulina powder[S]. Beijing: Standards Press of China, 1997.
    [14]
    中华人民共和国国家卫生和计划生育委员会. GB 19643-2016 食品安全国家标准 藻类及其制品[S]. 北京: 中国标准出版社, 2016.

    National Health and Family Planning Commission of the P. R. C. GB 19643-2016 National food safety standard algae and algae products[S]. Beijing: Standards Press of China, 2016.
    [15]
    JOHNNA A B, JUDY A W, GRACE M O, et al. Comparative analysis of microcystin prevalence in Michigan lakes by online concentration LC/MS/MS and ELISA[J]. Toxins,2019,11(1):13. doi: 10.3390/toxins11010013
    [16]
    LU N, LI L, GUAN T, et al. Broad-specificity ELISA with a heterogeneous strategy for sensitive detection of microcystins and nodularin[J]. Toxicon,2020,175:44−48. doi: 10.1016/j.toxicon.2019.12.003
    [17]
    许慧, 江敏, 王婧. 反相高效液相色谱法检测鲫鱼组织中的节球藻毒素[J]. 分析测试学报,2015,34(9):1072−1076. [XU H, JIANG M, WANG J. Determination of nodularin in Carassius auratus tissues by reversed phase high performance liquid chromatography[J]. Journal of Instrumental Analysis,2015,34(9):1072−1076. doi: 10.3969/j.issn.1004-4957.2015.09.016
    [18]
    MARYAM H, CARMEN T C, FRANCISCO J L, et al. Monitoring of cyanotoxins in water from hypersaline microalgae colonies by ultra high performance liquid chromatography with diode array and tandem mass spectrometry detection following salting-out liquid-liquid extraction[J]. Journal of Chromatography A,2019,1608:460409. doi: 10.1016/j.chroma.2019.460409
    [19]
    姜蕾, 张东. 高效液相色谱-串联质谱法同时分析水中9种典型藻毒素[J]. 给水排水,2013,39(6):37−41. [JIANG L, ZHANG D. Simultaneous determination of nine cyanotoxins in water by high performance liquid chromatography-tandem mass spectrometry[J]. Water and Wastewater Engineering,2013,39(6):37−41. doi: 10.3969/j.issn.1002-8471.2013.06.008
    [20]
    张秀尧, 蔡欣欣, 张晓艺, 等. 直接进样-超高效液相色谱-三重四极杆质谱法同时快速测定水中12种微囊藻毒素和1种节球藻毒素[J]. 色谱,2017,35(12):1286−1293. [ZHANG X Y, CAI X X, ZHANG X Y, et al. Simultaneous rapid determination of 12 microcystins and one nodularin in water by direct injection-ultra performance liquid chromatography-triple quadrupole mass spectrometry[J]. Chinese Journal of Chromatography,2017,35(12):1286−1293. doi: 10.3724/SP.J.1123.2017.09002
    [21]
    何海波, 时肖宁, 刘敏. 水体中微囊藻毒素和节球藻毒素的UPLC-MSn分析方法研究[J]. 环境与职业医学,2010,25(10):626−629. [HE H B, SHI X N, LIU M. Analysis of microcystins and nodularin in water by ultra performance liquid chromatography/tandem mass spectrometry[J]. Journal of Environmental and Occupational Medicine,2010,25(10):626−629.
    [22]
    沈斐, 许燕娟, 姜晟, 等. 超高效液相色谱-串联质谱法快速测定地表水中9种藻毒素[J]. 理化检验(化学分册),2018,54(11):1287−1291. [SHEN F, XU Y J, JIANG S, et al. Rapid determination of 9 algal toxins in surface water by UHPLC-MS/MS[J]. Physical Testing and Chemical Analysis Part B:Chemical Analysis,2018,54(11):1287−1291.
    [23]
    GIORGIA D P, GABRIELE F, FEDERICA N D G, et al. Multi-residue ultra performance liquid chromatography-high resolution mass spectrometric method for the analysis of 21 cyanotoxins in surface water for human consumption[J]. Talanta,2020,211:120738. doi: 10.1016/j.talanta.2020.120738
    [24]
    ZHANG H Y, GERARD BRYAN G, NATALIA V B, et al. Development of a validated direct injection-liquid chromatographic tandem mass spectrometric method under negative electro-spray ionization for quantitation of nine microcystins and nodularin-R in lake water[J]. Journal of Chromatography A,2020,1609:460432. doi: 10.1016/j.chroma.2019.460432
    [25]
    CRISTINA L, CLARA B, EDUARDO B, et al. Study of cyanotoxin degradation and evaluation of their transformation products in surface waters by LC-QTOF MS[J]. Chemosphere,2019,229:538−548. doi: 10.1016/j.chemosphere.2019.04.219
    [26]
    TURNER A D, WAACK J, LEWIS A, et al. Development and single-laboratory validation of a UHPLC-MS/MS method for quantitation of microcystins and nodularin in natural water, cyanobacteria, shellfish and algal supplement tablet powders[J]. Journal of Chromatography B,2018,1074-1075:111−123. doi: 10.1016/j.jchromb.2017.12.032
    [27]
    GIMÉNEZ-CAMPILLO C, PASTOR-BELDA M, CAMPILLO N, et al. Determination of cyanotoxins and phycotoxins in seawater and algae-based food supplements using ionic liquids and liquid chromatography with time-of-flight mass spectrometry[J]. Toxins,2019,11(10):610. doi: 10.3390/toxins11100610
    [28]
    陈丽惠, 贾玉珠, 张斌, 等. 分散固相萃取-液相色谱-串联质谱法测定淡水鱼中柱孢藻毒素、节球藻毒素和微囊藻毒素[J]. 色谱,2019,37(7):723−728. [CHEN L H, JIA Y Z, ZHANG B, et al. Determination of cylindrospermopsin, nodularin and microcystins in freshwater fish by dispersive solid phase extraction- liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography,2019,37(7):723−728. doi: 10.3724/SP.J.1123.2019.01022
    [29]
    虞锐鹏, 陶冠军, 杨健, 等. 超高效液相色谱-四极杆-飞行时间质谱法快速测定水产品中微囊藻毒素和节球藻毒素[J]. 分析试验室,2012,31(1):80−83. [YU R P, TAO G J, YANG J, et al. Determination of microcystins and nodularins in aquatic products by ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry[J]. Chinese Journal of Analysis Laboratory,2012,31(1):80−83. doi: 10.3969/j.issn.1000-0720.2012.01.019
    [30]
    金玉娥, 汪国权, 马佳鸣, 等. 高效液相色谱-串联质谱法同时测定水产品中7种微囊藻毒素[J]. 环境与职业医学,2012,29(6):343−346. [JIN Y E, WANG G Q, MA J M, et al. Determination of 7 microcystin variants in aquatic products by high performance liquid chromatography tandem triple quadrupole mass spectrometry[J]. Journal of Environmental and Occupational Medicine,2012,29(6):343−346.
    [31]
    SAMUEL P H, JONATHAN M B, RAEGYN B T, et al. Determination of microcystins, nodularin, anatoxin-a, cylindrospermopsin, and saxitoxin in water and fish tissue using isotope dilution liquid chromatography tandem mass spectrometry[J]. Journal of Chromatography A,2019,1599:66−74. doi: 10.1016/j.chroma.2019.03.066
    [32]
    黄会, 刘慧慧, 李佳蔚, 等. 水产品中微囊藻毒素检测方法及污染状况研究进展[J]. 中国渔业质量与标准,2019,9(2):32−43. [HUANG H, LIU H H, LI J W, et al. Progress on study of detection methods and pollution condition of microcystins in aquatic products[J]. China Fishery Quality and Standards,2019,9(2):32−43. doi: 10.3969/j.issn.2095-1833.2019.02.005
  • Related Articles

    [1]LIU Zhong, ZHANG Zheng, LOU Xuyang, ZHU Jinlin. Quality-related and Quality-irrelevant Fault Detection and Diagnosis in Batch Fermentation Process Based on NSSAE[J]. Science and Technology of Food Industry. DOI: 10.13386/j.issn1002-0306.2024020300
    [2]ZHANG Yusong, CUI Weiran, TANG Zhenyue, BAI Hongyu, SHAO Meili. Effects of Whey Protein Concentrate on the Bioaccessibility and Microstructure of 5-Methyltetrahydrocalcium Folate in a Simulated Digestive Environment in Vitro[J]. Science and Technology of Food Industry. DOI: 10.13386/j.issn1002-0306.2024010302
    [3]ZHANG Quantong, ZHENG Yao, YANG Liu, ZHANG Shuaishuai, GUO Quanyou. Rapid Detection of Astaxanthin in Antarctic Krill Meal by Computer Vision Combined with Convolutional Neural Network[J]. Science and Technology of Food Industry. DOI: 10.13386/j.issn1002-0306.2024030200
    [4]XIAO Chunyan, LI Jing, WANG Zhihui, HE Biyun, HUANG Wei, LIN Fuming, CHEN Linhai, SUN Weijiang. Analysis of Flavor and Quality Differences in Black Tea from Different Geographical Origins in Fujian[J]. Science and Technology of Food Industry. DOI: 10.13386/j.issn1002-0306.2024030491
    [5]ZHU Kai, DING Zhuoyi, WU Yifei, LIU Zhiquan, DUAN Xiaoquan, ZHANG Zhuqing, CHEN Wenchao, LIAO Luyan, ZHOU Xiaobo. Composition and Comprehensive Evaluation of Free Amino Acids in Different Brassica Campestris Cultivars[J]. Science and Technology of Food Industry. DOI: 10.13386/j.issn1002-0306.2024030348
    [6]WANG Shengyu, HUANG Yousheng, CHEN Lihua, DONG Huanhuan, GUAN Yongmei, ZHU Weifeng. Effects of Solid Fermentation of Aspergillus Niger on Release of Conjugated Phenolics and Antioxidant Activity of By-products of Pueraria Thomsonii[J]. Science and Technology of Food Industry. DOI: 10.13386/j.issn1002-0306.2024030344
  • Cited by

    Periodical cited type(2)

    1. 西尔力·阿不都热哈曼,何晓露,庞润涛,刘河疆. 不同地区枸杞真菌毒素含量特征分析. 食品安全质量检测学报. 2024(17): 92-100 .
    2. 黄康惠,卢鑫,周璇,王文富,杨福兴,朱桂芳,孙宇. 高效液相色谱串联质谱法测定食品中双丙酚丁等致泻药物. 食品科技. 2023(06): 301-307 .

    Other cited types(1)

Catalog

    Article Metrics

    Article views (172) PDF downloads (13) Cited by(3)

    /

    DownLoad:  Full-Size Img  PowerPoint
    Return
    Return