高分辨四极杆飞行时间质谱仪判别复原乳和超高温灭菌乳
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摘要
采用高分辨四极杆飞行时间质谱仪,结合化学计量学方法,利用非靶向代谢组学方法,对超高温灭菌乳和复原乳进行检测。牛乳样品经过前处理后,经过C18色谱柱分离,采用FullScan模式进行一级全扫描,扫描结果通过数据预处理后,导入SIMCA-P14.1软件中进行主成分分析和偏最小二乘方差判别分析。结果表明:正、负离子模式下共找到14种判别超高温灭菌乳和复原乳的表征因子,进一步通过这14种表征因子建立区分2种乳的判别模型,通过该判别模型能够准确地区分超高温灭菌乳和复原乳,为复原乳的判别提供理论依据。
In this study, ultra-high temperature (UHT) milk and reconstituted milk were discriminated by high resolution quadrupole-time of flight mass spectrometry (LC-Q-TOF-MS) combined with chemometrics based on non-targeted metabolomic approaches. Sample pretreatment was performed prior to chromatographic separation on a C18 column, and the mass spectrometer was operated in the full scan mode. The obtained data were preprocessed before being imported into SIMCA-P 14.1 for principal component analysis (PCA) and partial least squares-discrimination analysis (PLS-DA). A total of 14 characterization factors were selected in both positive and negative ion modes to establish a discriminant model. The results showed that this model could be used as a robust approach to discriminate between UHT and reconstituted milk and provide a theoretical basis for the identification of reconstituted milk.
In this study, ultra-high temperature (UHT) milk and reconstituted milk were discriminated by high resolution quadrupole-time of flight mass spectrometry (LC-Q-TOF-MS) combined with chemometrics based on non-targeted metabolomic approaches. Sample pretreatment was performed prior to chromatographic separation on a C18 column, and the mass spectrometer was operated in the full scan mode. The obtained data were preprocessed before being imported into SIMCA-P 14.1 for principal component analysis (PCA) and partial least squares-discrimination analysis (PLS-DA). A total of 14 characterization factors were selected in both positive and negative ion modes to establish a discriminant model. The results showed that this model could be used as a robust approach to discriminate between UHT and reconstituted milk and provide a theoretical basis for the identification of reconstituted milk.
引文
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[22]柯朝甫,张涛,武晓岩,等.代谢组学数据分析的统计学方法[J].中国卫生统计,2014,31:357-359.
[23]王中华.基于代谢组学的2型糖尿病和环境污染物暴露生物标志物研究[D].北京:北京协和医学院,2015.
[24]MORTIER L,BRAEKMAN A,CARTUYVELS D,et al.Intrinsic indicators for monitoring heat damage of consumption milk[J].Biotechnologie Agronomie Societe Et Environnement,2000,4(4):221-225.
[2]SIKAND V,TONG P S,WALIKER J.Heat stability of reconstituted,protein-standardized skim milk powders[J].Journal of Dairy Science,2010,93(12):5561-5571.DOI:10.3168/jds.2010-3128.
[3]付洪涛,欧阳华学,雷绍荣.高效液相色谱法测定复原乳中糠氨酸的含量[J].中国测试,2008,34(2):103-104; 137.
[4]CHO Y H, HONG S M,KIM C H.Determination of lactulose and furosine formation in heated milk as a milk quality indicator[J].Korean Journal for Food Science of Animal Resources,2012,32(5):540-544.DOI:10.5851/kosfa.2012.32.5.540.
[5]MONTILLA A,CALVO M M,SANTA-MARIA G,et al.Correlation between lactulose and furosine in UHT-heated milk[J].Journal of Food Protection,1996,59(10):1061-1064.DOI:10.4315/0362-028X-59.10.1061.
[6]PAPPAS C S,SAKKAS L,MOSCHOPOULOU E,et al.Direct determination of lactulose in heat-treated milk using diffuse reflectance infrared Fourier transform spectroscopy and partial least squares regression[J].International Journal of Dairy Technology,2015,68(3):448-453.DOI:10.1111/1471-0307.12233.
[7]CALVANO C D,MONOPOLI A,LOIZZO P,et al.Proteomic approach based on MALDI-TOF MS to detect powdered milk in fresh cow's milk[J],Journal of Agricultural and Food Chemistry,2013,61(8):1609-1617.DOI:10.1021/jf302999s.
[8]钱宇,汪慧超,吴林昊,等.超高效液相色谱检测乳粉复原乳中的氨基酸[J].食品与机械,2016,32(7):56-60.DOI:10.13652/j.issn.1003-5788.2016.07.013.
[9]姜全忠,周红,陶大利,等.离子色谱法测定UHT灭菌乳中的乳果糖在复原乳鉴定中的应用[J].中国乳品工业,2016,44(4):48-51.DOI:10.3969/j.issn.100 1-2230.2016.04.013.
[10]BLOCK J D,MERCHIERS M,RENTERGHEM R V,et al.Evaluation of two methods for the determination of lactulose in milk[J].International Dairy Journal,1996,6(2):217-222.DOI:10.1016/0958-6946(95)00006-2.
[11]AMINE A,MOSCONE D,BERNARDO R A.A new enzymatic spectrophotometric assay for the determination of lactulose in milk[J].Analytica Chimica Acta,2000,406(2):217-224.DOI:10.1016/S0003-2670(99)00765-5.
[12]中华人民共和国农业部.巴氏杀菌乳和UHT灭菌乳中复原乳的鉴定:NY/T 939-2016[S].北京:中国农业出版社,2016.
[13]MARCONI E,MESSIA M C,AMINE A,et al.Heat-treated milk differentiation by a sensitive lactulose assay[J].Food Chemistry,2004,84(3):447-450.DOI:10.1016/S0308-8146(03)00268-1.
[14]SAKKAS L,MOUTAFI A,MOSCHOPOULOU E,et al.Assessment of heat treatment of various types of milk[J].Food Chemistry,2014,159:293-301.DOI:10.1016/j.foodchem.2014.03.020.
[15]THERESE J,CLAUSEN M R, SUNDEKILDE U K,et al.Lactosehydrolyzed milk is more prone to chemical changes during storage than conventional ultra-high-temperature(UHT)milk[J].Journal of Agricultural and Food Chemistry,2014,62(31):7886-7896.D01:10.1021/jf501671z.
[16]YOUNG K J,YEON P J,OH YOEN K,et al.Metabolic profiling of plasma in overweight/obese and lean men using ultra performance liquid chromatography and Q-TOF mass spectrometry(UPLC-QTOF MS)[J].Journal of Proteome Research,2010,9(9):4368-4375.DOI:10.1021/pr100101p.
[17]ZHAO Y Y,LIU J, CHENG X L,et al.Urinary metabonomics study on biochemical changes in an experimental model of chronic renal failure by adenine based on UPLC Q-TOF/MS[J].Clinica Chimica Acta,2012,413(5/6):642-649.DOI:10.101 6/j.cca.201 1.12.014.
[18]FARAG M A,EL-AHMADY S H,ELIAN F S,et al.Metabolomics driven analysis of artichoke leaf and its commercial products via UHPLC-Q-TOF-MS and chemometrics[J].Phytochemistry,2013,95:1 77-187.DOI:10.101 6/j.phytochem.2013.07.003.
[19]LUBES G,GOODARZI M.Analysis of volatile compounds by advanced analytical techniques and multivariate chemometrics[J].Chemical Reviews,2017,1 17(9):6399-6422.DOI:10.102 1/acs.chemrev.6b00698.
[20]MAIS E,ALOLGA R N,WANG S L,et al.A comparative UPLC-Q/TOF-MS-based metabolomics approach for distinguishing Zingiber officinale Roscoe of two geographical origins[J].Food Chemistry,2017,240:239-244.DOI:10.1016/j.foodchem.2017.07.106.
[21]ZHAO Qiqi,ZHANG Aihua,ZONG Wenjing,et al.Chemometrics strategy coupled with high resolution mass spectrometry for analyzing and interpreting comprehensive metabolomic characterization of hyperlipemia[J].RSC Advances,2016(6):112534-112543.DOI:10.1039/C6RA24267G.
[22]柯朝甫,张涛,武晓岩,等.代谢组学数据分析的统计学方法[J].中国卫生统计,2014,31:357-359.
[23]王中华.基于代谢组学的2型糖尿病和环境污染物暴露生物标志物研究[D].北京:北京协和医学院,2015.
[24]MORTIER L,BRAEKMAN A,CARTUYVELS D,et al.Intrinsic indicators for monitoring heat damage of consumption milk[J].Biotechnologie Agronomie Societe Et Environnement,2000,4(4):221-225.