Determination of 4 Kinds of Frequently-used Spices in Dairy Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

LIN Zhengfeng; LI Shifei; HUANG Jieying; XUAN Kaizhi; WANG Chaozheng

doi:10.13386/j.issn1002-0306.2021010170

Volume 42 Issue 21

Oct. 2021

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Science and Technology of Food Industry > 2021 > 42(21): 271-278. > DOI: 10.13386/j.issn1002-0306.2021010170

LIN Zhengfeng, LI Shifei, HUANG Jieying, et al. Determination of 4 Kinds of Frequently-used Spices in Dairy Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(21): 271−278. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021010170.

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Determination of 4 Kinds of Frequently-used Spices in Dairy Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

Haikou Customs District People’ s Republic of China Technology Center, Haikou 570311, China

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Received Date: January 20, 2021
Available Online: August 29, 2021

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Abstract

Abstract

An analytical method based on high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed for detecting 4 kinds of frequently-used spices (maltol, ethyl-maltol, vanillin and ethyl-vanillin) in dairy products. The samples were extracted by water and tert butyl methyl ether, the supernatants were extracted by 0.2 mol/L sodium hydroxide solution alkali solution (the volume ratio of alkali solution to MTBE was 1:5) for purification and enrichment of target composes to the aqueous phase. The separation of these 4 compounds was carried out by a HSS T3 column and the mobile phase performed on 0.05% formic acid aqueous solution-methanol by gradient elution, electrospray ionization source (ESI) was applied and operated in the positive mode. Multiple reaction monitoring (MRM) mode was used to monitor ions. The results showed that the method had a good linearity range between 2.0~100.0 ng/mL (R²>0.995) and the detection limits were as low as 8.0 μg/kg. The matrix effects of 4 kinds of spices in different dairy products showed week matrix suppression effects and ranged from 80%~100%, suggesting the matrix effects advisably being ignored in routine testing. The average recoveries of the targeted compounds range from 67.7% to 104.8% at spiked levels of 10, 25 and 100 μg /kg, and relative standard deviations range from 2.5% to 11.9% (n=6). The method is simple, sensitive, accurate and reliable.
- dairy products,
- maltol,
- ethyl-maltol,
- vanillin,
- ethyl-vanillin,
- high performance liquid chromatography-tandem mass spectrometry

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References

[1]	Khan I T, Nadeem M, Imran M, et al. Antioxidant properties of milk and dairy products: A comprehensive review of the current knowledge[J]. Lipids in Health and Disease,2019,18:41−53. doi: 10.1186/s12944-019-0969-8
[2]	蒋慧, 田洪芸, 田栋, 等. 近三年婴幼儿配方乳粉质量状况及相关监管要求[J]. 中国乳品工业,2018,46(4):39−42. [Jiang H, Tian H Y, Tian D, et al. Quality status of infant formula milk powder in recent three years and related regulatory requirements[J]. China Dairy Industry,2018,46(4):39−42. doi: 10.3969/j.issn.1001-2230.2018.04.009
[3]	Fu X, Zhu D L, Huang L, et al. Superparamagnetic core-shell dummy template molecularly imprinted polymer for magnetic solid-phase extraction of food additives prior to the determination by HPLC[J]. Microchemical Journal, 2019, 150, 104169.
[4]	穆旻, 郑福平, 孙宝国, 等. 麦芽酚和乙基麦芽酚的合成及其在食品工业中的应用[J]. 中国食品学报,2006,6(1):407−410. [Mu M, Zheng F P, Sun B G, et al. Synthesis of maltol and ethyl maltol and their application in food industry[J]. Journal of Chinese Institute of Food Science and Technology,2006,6(1):407−410. doi: 10.3969/j.issn.1009-7848.2006.01.084
[5]	陈荣荣, 许耀伟, 郭宁, 等.一种牛奶香精配方: 中国, 201310655903.9[P]. 2016-08-17. Chen R R, Xu Y W, Guo N, et al. A formula for milk flavor: CN 201310655903.9[P]. 2016-08-17.
[6]	司晓晶, 韩婧婷, 朱文菁, 等.石墨烯/四氧化三钴电化学传感器的建立及检测香兰素[J/OL].食品工业科技. https://doi.org/10.13386/j.issn1002-0306.2020040287. Si X J, Han J T, Zhu W J, et al. Establishment of graphene/cobaltosic cxide electrochemical sensor and the detection of vanillin[J/OL]. Science and Technology of Food Industry. https://doi.org/10.13386/j.issn1002-0306.2020040287.
[7]	Zhao J, Xia H X, Yu T Y, et al. A colorimetric assay for vanillin detection by determination of the luminescence of o-toluidine condensates[J]. PloS One,2018,13(4):e0194010. doi: 10.1371/journal.pone.0194010
[8]	程雷, 孙宝国, 宋焕禄, 等. 食用香精香料的安全性评价现状及发展趋势[J]. 食品科学,2010,31(21):409−412. [Cheng L, Sun B G, Song H L, et al. Current research and trend of safety evaluation of food flavorings[J]. Food Science,2010,31(21):409−412.
[9]	王玉娇, 邓伟, 刘通, 等. 食品中香料香精分析方法研究进展[J]. 食品安全质量检测学报,2019,10(2):400−406. [Wang Y J, Deng W, Liu T, et al. Research progress of detection techniques for food flavors and fragrances[J]. Journal of Food Safety and Quality,2019,10(2):400−406. doi: 10.3969/j.issn.2095-0381.2019.02.020
[10]	中华人民共和国国家卫生和计划生育委员会.GB 2760-2014: 食品安全国家标准食品添加剂使用标准 [S].北京: 中国标准出版社, 2014. National Health and Family Planning Commission of the People's Republic of China. GB2760-2014: National food safety standard, standard for uses of food additives[S]. Beijing: Standards Press of China, 2014.
[11]	Ni Y N, Zhang G W, Kokot S. Simultaneous spectrophotometric determination of maltol, ethyl maltol, vanillin and ethyl vanillin in foods by multivariate calibration and artificial neural networks[J]. Food Chemistry,2005,89(3):465−473. doi: 10.1016/j.foodchem.2004.05.037
[12]	Ma Y J, Bi A Q, Wang X Y, et al. Dispersive solid-phase extraction and dispersive liquid-liquid microextraction for the determination of flavor enhancers in ready-to-eat seafood by HPLC-PDA[J]. Food Chemistry,2020,309:125753. doi: 10.1016/j.foodchem.2019.125753
[13]	迟秋池, 李晓雯, 何家今, 等. 高效液相色谱法同时测定豆浆中麦芽酚、乙基麦芽酚、香兰素、甲基香兰素和乙基香兰素5种香料[J]. 食品安全质量检测学报,2016,7(7):2690−2695. [Chi Q C, Li X W, He J J, et al. Simultaneous determination of maltol, ethyl maltol, vanillin, methyl vanillin and ethyl vanillin in soya bean milk by high performance liquid chromatography[J]. Journal of Food Safety and Quality,2016,7(7):2690−2695.
[14]	Ma J, Zhang B, Wang Y N, et al. Determination of flavor enhancers in milk powder by one-step sample preparation and two-dimensional liquid chromatography[J]. Journal of Separation Science,2014,37:920−926. doi: 10.1002/jssc.201301367
[15]	Peng J F, Wei M L, Hu Y W, et al. Simultaneous determination of maltol, ethyl maltol, vanillin, and ethyl vanillin in foods by isotope dilution headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry[J]. Food Analytical Methods,2019,12(8):1725−1735. doi: 10.1007/s12161-019-01518-3
[16]	杨华梅, 杭莉. 超高效液相色谱-串联质谱法同时测定食品中4种常用香精[J]. 色谱,2015,33(3):250−255. [Yang H M, Hang L, et al. Determination of four frequently-used essences in foods by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography,2015,33(3):250−255. doi: 10.3724/SP.J.1123.2014.11018
[17]	宁霄, 何欢, 金绍明, 等. 超高效液相色谱-串联质谱法同时测定食品中麦芽酚、乙基麦芽酚、香兰素、甲基香兰素和乙基香兰素[J]. 食品安全质量检测学报,2017,8(7):2555−2562. [Ning X, He H, Jin S M, et al. Simultaneous determination of vanillin, methyl vanillin, ethyl vanillin, maltol and ethyl maltol in foods by ultra performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety and Quality,2017,8(7):2555−2562. doi: 10.3969/j.issn.2095-0381.2017.07.028
[18]	韩超, 刘滨, 朱振瓯, 等. 液相色谱-串联质谱法同时测定婴幼儿配方奶粉中4种香料[J]. 分析测试学报,2013,33(2):208−211. [Han C, Liu B, Zhu Z O, et al. Simultaneous determination of 4 spice in infant formula samples by liquid chromatography-tandem mass spectrometry[J]. Journal of Instrumental Analysis,2013,33(2):208−211.
[19]	罗冠中, 刘祥, 孟云彩. 液相色谱串联四极杆质谱法同时测定婴幼儿配方食品中甲基香兰素和乙基香兰素[J]. 分析试验室,2011,30(8):84−87. [Luo G Z, Liu X, Meng Y C. Simultaneous determination of methyl vanillin and ethyl vanillin in infant formula milk powder by liquid chromatography-tandem mass spectrometry[J]. Journal of Instrumental Analysis,2011,30(8):84−87. doi: 10.3969/j.issn.1000-0720.2011.08.021
[20]	曲宝成, 戴学东, 张敬波, 等. 高效液相色谱串联质谱法测定植物油中香兰素、甲基香兰素和乙基香兰素[J]. 食品安全质量检测学报,2018,9(4):935−941. [Qu B C, Dai X D, Zhang J B, et al. Determination of vanillin, methyl vanillin and ethyl vanillin in vegetable oil by high performance liquid chromatography tandem mass spectrometry[J]. Journal of Food Safety and Quality,2018,9(4):935−941. doi: 10.3969/j.issn.2095-0381.2018.04.042
[21]	吴纤愫, 郑平安, 周勇, 等. 不同种类固相萃取柱对特医食品中香料含量结果的影响[J]. 食品工业,2021,42(1):291−296. [Wu Q S, Zheng P A, Zhou Y, et al. Effect of different kinds of SPE columns on the results of flavor content in special medical foods[J]. The Food Industry,2021,42(1):291−296.
[22]	杨丽莉, 王美飞, 胡恩宇, 等. 超声波提取-气相色谱法测定土壤中21种酚类化合物[J]. 色谱,2013,31(11):1081−1086. [Yang L L, Wang M F, Hu E Y, et al. Determination of 21 phenolic compouds in soil by ultrasonic extraction-gas chromatograhy[J]. Chinese Journal of Chromatography,2013,31(11):1081−1086. doi: 10.3724/SP.J.1123.2013.05005
[23]	钟惠英, 柳海, 柴丽月, 等. 气相色谱-质谱法测定水产品中19种氯代酚及其钠盐[J]. 分析科学学报,2016,32(3):371−376. [Zhong H Y, Liu H, Chai L Y, et al. Determination of 19 chlorophenols and their sodium salts by gas chromatograhy-mass spectrometry in aquatic products[J]. Journal of Analytical Science,2016,32(3):371−376. doi: 10.2116/analsci.32.371
[24]	林仙军, 罗成江, 周志强, 等. UPLC法测定鳗鱼和甲鱼诱食剂中乙基麦芽酚和香兰素[J]. 饲料研究,2013,9:81−84. [Lin X J, Luo C J, Zhou Z Q, et al. Determination of ethyl maltol and vanillin in food attractants for eel and turtle bait by UPLC[J]. Feed Research,2013,9:81−84. doi: 10.3969/j.issn.1002-2813.2013.04.026
[25]	章建辉, 李莎, 黄辉, 等. 液液萃取-接受相固化-反萃取-气相色谱/质谱法测定奶粉中的香兰素[J]. 食品与机械,2015,31(2):98−101, 105. [Zhang J H, Li S, Huang H, et al. Determination of vanillin in powdered milk by liquid-liquid extraction-solidification of acceptor phase-reextraction-gas chromatography/mass spectrometry[J]. Food & Machinery,2015,31(2):98−101, 105.
[26]	许文娟, 王振刚, 丁葵英, 等. QuEChERS/液相色谱-串联质谱法测定5种蔬菜中17种氨基甲酸酯类农药的基质效应研究[J]. 分析测试学报,2017,36(1):54−60. [Xu W J, Wang Z G, Ding K Y, et al. Detection of matrix effects of 17 carbamate pesticides in 5 vegetables by QuEChERS/LC-MS /MS method[J]. Journal of Instrumental Analysis,2017,36(1):54−60.
[27]	Kojro G, Rudzki P J, Pisklak D M, et al. Matrix effect screening for cloud-point extraction combined with liquid chromatography coupled to mass spectrometry: Bioanalysis of pharmaceuticals[J]. Journal of Chromatography A,2019,1591:44−54. doi: 10.1016/j.chroma.2019.01.031
[28]	中华人民共和国国家质量监督检验检疫总局, 中国国家标准化管理委员会. GB/T 27404-2008 实验室质量控制规范食品理化检验[S]. 北京: 中国标准出版社, 2008. The Standardization Administration of China, General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China. GB/T 27404-2008 Criterion on quality control of laboratories-chemical testing of food[S]. Beijing: Standards Press of China, 2008.
[29]	赵雁冰, 顾娅楠, 杨恒, 等. UPLC-DAD测定奶粉中5种香精含量[J]. 当代化工研究,2020(13):157−158. [Zhao Y B, Gu Y N, Yang H, et al. UPLC-DAD determination of five essences in milk powder[J]. Modern Chemical Research,2020(13):157−158. doi: 10.3969/j.issn.1672-8114.2020.13.073
[30]	中华人民共和国国家卫生部.GB 19302-2010: 食品安全国家标准发酵乳[S].北京: 中国标准出版社, 2010. Ministry of Health of the People's Republic of China. GB19302–2010 National food safety standard, fermented milk [S]. Beijing: Standards Press of China, 2010.
[31]	Jo Y, Benoist D M, Barbano D M, et al. Flavor and flavor chemistry differences among milks processed by high temperature, short time or ultra-pasteurization[J]. Journal of Dairy Science,2018,101(5):3812−3828. doi: 10.3168/jds.2017-14071
[32]	Su X Q, Tortorice M, Ryo S, et al. Sensory lexicons and formation pathways of off-aromas in dairy ingredients: A review[J]. Molecules,2020,25(3):569. doi: 10.3390/molecules25030569