高效液相色谱法测定果汁、果酱中的皂黄
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摘要
目的建立高效液相色谱法检测果汁、果酱中皂黄含量的分析方法。方法试样经20%(V:V)甲醇溶液超声提取,离心取上清液,高效液相色谱—二极管阵列检测器分析。结果皂黄在0.50～100μg/mL浓度范围内呈现良好的线性关系(r~2>0.9999),具有较高的分离度且峰型对称,果汁和果酱的标准物质加入实验的回收率分别在96.1%～101.9%和79.2%～99.4%之间,相对标准偏差(relative standard deviation,RSD)分别为1.1%～2.3%和4.3%～7.4%。结论该方法具有操作简便、准确度高、灵敏度高和稳定性好等优点,适用于果汁、果酱中皂黄含量的测定。
Objective To establish a method for the determination of the content of metanil yellow in juice and jam by high performance liquid chromatography(HPLC). Methods The samples were ultrasonically extracted in 20%(V:V) methanol solution, the supernatant after centrifuging was analyzed by high performance liquid chromatography-diode array detector(HPLC-DAD). Results Metanil yellow had good linear relationships in the range of 0.50-100 μg/mL, r~2>0.9999. The recoveries of metanil yellow in juice and jam samples were 96.1%-101.9% and 79.2%-99.4%, respectively, with the relative standard deviations of 1.1%-2.3% and 4.3%-7.4%. Conclusion This method had the advantages of easy operating, high sensitivity, high accuracy and good stability, which is suitable for the detection of metanil yellow in juice and jam.
Objective To establish a method for the determination of the content of metanil yellow in juice and jam by high performance liquid chromatography(HPLC). Methods The samples were ultrasonically extracted in 20%(V:V) methanol solution, the supernatant after centrifuging was analyzed by high performance liquid chromatography-diode array detector(HPLC-DAD). Results Metanil yellow had good linear relationships in the range of 0.50-100 μg/mL, r~2>0.9999. The recoveries of metanil yellow in juice and jam samples were 96.1%-101.9% and 79.2%-99.4%, respectively, with the relative standard deviations of 1.1%-2.3% and 4.3%-7.4%. Conclusion This method had the advantages of easy operating, high sensitivity, high accuracy and good stability, which is suitable for the detection of metanil yellow in juice and jam.
引文
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[10]翟海云,刘振平,何建英,等.高效液相色谱法同时测定黄花鱼中4种禁用黄色工业染料[J].理化检验(化学分册),2013,49(9):1110-1113.Zhai HY,Liu ZP,He JY,et al.Simultaneous determination of 4 contraband yellow industrial dyes in yellow croaker by HPLC[J].Phys Test Chem Anal B,2013,49(9):1110-1113.
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[13]Guo X,Wei Q,Du B,et al.Removal of metanil yellow from water environment by amino functionalized graphenes(NH2-G)-Influence of surface chemistry of NH2-G[J].Appl Surface Sci,2013,284(10):862-869.
[14]Mittal A,Gupta VK,Malviya A,et al.Process development for the batch and bulk removal and recovery of a hazardous,water-soluble azo dye(metanil yellow)by adsorption over waste materials(bottom ash and de-oiled soya)[J].J Hazard Mater,2008,151(2):821-832.
[15]Fuh MR,Chia KJ.Determination of sulphonated azo dyes in food by ionpair liquid chromatography with photodiode array and electrospray mass spectrometry detection[J].Talanta,2002,56:663-671.
[16]夏立娅,韩媛媛,匡林鹤,等.薄层色谱扫描法同时检测豆制品中碱性橙、皂黄、柠檬黄和日落黄以及辣椒粉中酸性橙Ⅱ、丽春红2R和罗丹明B[J].分析试验室,2010,29(6):15-18.Xia LY,Han YY,Kuang LH,et al.Simultaneous determination of basic orangeⅡ,metanil yellow,tartrazine,sunset yellow in bean-product and acid orangeⅡ,ponceau 2R,rhodanmine B in chili powder by thin-layer chromatographic scanning[J].Chin J Anal Lab,2010,29(6):15-18.
[17]吴彦蕾,林晓洋,胡靖,等.高效液相色谱法快速检测食品中18种合成色素[J].食品工业科技,2013,34(24):49-52.Wu YL,Lin XY,Hu J,et al.Fast determination of 18 synthetic colors in foods by high performance liquid chromatography[J].Sci Technol Food Ind,2013,34(24):49-52.
[18]刘杰,王占利,张先聚,等.果汁果酱与乳制品中苯甲酸、山梨酸同步检测实验[J].中国奶牛,2014,(19):29-31.Liu J,Wang ZL,Zhang XJ,et al.Simultaneous determination of benzoic acid and sorbic acid in fruit juice and jam and dairy products[J].China Dairy Cattle,2014,(19):29-31.
[19]GB/T 27404-2008实验室质量控制规范食品理化检测[S].GB/T 27404-2008 Criterion on quality control of laboratories-Chemical testing of food[S].
[20]赵灵芝,刘春叶,王海洋,等.高效液相色谱法测定硝苯地平片含量的方法学研究[J].化学与生物工程,2014,31(07):70-72.Zhao LZ,Liu CY,Wang HY,et al.The methodological study for HPLCdetermination of nifedipine content[J].Chem Bioeng,2014,31(7):70-72.
[21]崔连喜,张肇元,吴宇峰,等.样品溶剂对高效液相色谱分析结果的影响[J].广州化工,2016,44(18):157-158.Cui LX,Zhang ZY,Wu YF,et al.Effect of sample solvent on HPLCanalysis results[J].Guangzhou Chem Ind,2016,44(18):157-158.
[2]赵志磊,吴广臣,李小亭,等.高效液相色谱测定食品中非食用色素皂黄[J].食品工业科技,2008,(6):284-285.Zhao ZL,Wu GC,Li XT,et al.Determination of metanil yellow in food by high performance liquid chromatography[J].Sci Technol Food Ind,2008,(6):284-285.
[3]Tural S,Tarhan T,Tural B.Removal of hazardous azo dye metanil yellow from aqueous solution by cross-linked magnetic biosorbent;equilibrium and kinetic studies[J].Desalinat Water Treatment,2016,57(28):13347-13356.
[4]闫正,张丽冰,任孟伟,等.表面增强激光拉曼光谱测定豆制品中的碱性嫩黄Ⅱ、碱性橙Ⅱ、皂黄[J].光谱学与光谱分析,2016,36(6):1761-1764.Yan Z,Zhang LB,Ren MW,et al.Fast determination of auramineⅡ,basic orangeⅡand metanil yellow in bean products on surface enhanced raman spectroscopy and use high pergormance liquid chromatography-tandem mass spectrometry to verify[J].Spectrosc Spectr Anal,2016,36(6):1761-1764.
[5]吴安波.一种pH精密试纸的制备方法:中国,CN 103033511 A[P].2014-10-29.Wu AB.The invention relates to a preparation method of pH precision test paper:CN 103033511 A[P].2014-10-29.
[6]张爱梅,王怀生,王术皓,等.溴酸钾氧化酸性间胺黄动力学光度法测定食品中微量碘[J].分析化学,1996,(6):689-691.Zhang AM,Wang HS,Wang SH,et al.Kinetic spectrophotometric determination of trace iodine in food by potassium bromate oxidation of interacid amine yellow[J].Chin J Anal Chem,1996,(6):689-691.
[7]张爱梅,王怀生,王术皓,等.藉溴酸钾氧化酸性间胺黄反应催化光度测定痕量亚硝酸根和硝酸根[J].分析化学,1996,(3):292-295.Zhang AM,Wang HS,Wang SH,et al.Catalytic spectrophotometric determination of trace nitrite and nitrite by potassium bromate oxidation of interacid amine yellow reaction[J].Chin J Anal Chem,1996,(3):292-295.
[8]金玉娥,孙丕,沈红,等.食品中违禁色素橙黄II和酸性间胺黄的HPLC测定研究[J].上海计量测试,2006,(4):19-21.Jin YE,Sun P,Shen H,et al.Research for determination of orangeⅡand metanil yellow in food by HPLC[J].Shanghai J Metrol Test,2006,(4):19-21.
[9]Khanna SK,Das M.Toxicity,carcinogenic potential and clinico-epidemiological studies on dyes and dye intermediates[J].J Sci Ind Res,1991,50:965-974.
[10]翟海云,刘振平,何建英,等.高效液相色谱法同时测定黄花鱼中4种禁用黄色工业染料[J].理化检验(化学分册),2013,49(9):1110-1113.Zhai HY,Liu ZP,He JY,et al.Simultaneous determination of 4 contraband yellow industrial dyes in yellow croaker by HPLC[J].Phys Test Chem Anal B,2013,49(9):1110-1113.
[11]Bonan S,Fedrizzi G,Menotta S,et al.Simultaneous determination of synthetic dyes in foodstuffs and beverages by high performance liquid chromatography coupled with diode-array detector[J].Dyes Pigment,2013,99(1):36-40.
[12]Feng F,Zhao Y,Yong W,et al.Highly sensitive and accurate screening of 40 dyes in soft drinks by liquid chromatography-electrospray tandem mass spectrometry[J].J Chromatogr B,2011,879(20):1813-1818.
[13]Guo X,Wei Q,Du B,et al.Removal of metanil yellow from water environment by amino functionalized graphenes(NH2-G)-Influence of surface chemistry of NH2-G[J].Appl Surface Sci,2013,284(10):862-869.
[14]Mittal A,Gupta VK,Malviya A,et al.Process development for the batch and bulk removal and recovery of a hazardous,water-soluble azo dye(metanil yellow)by adsorption over waste materials(bottom ash and de-oiled soya)[J].J Hazard Mater,2008,151(2):821-832.
[15]Fuh MR,Chia KJ.Determination of sulphonated azo dyes in food by ionpair liquid chromatography with photodiode array and electrospray mass spectrometry detection[J].Talanta,2002,56:663-671.
[16]夏立娅,韩媛媛,匡林鹤,等.薄层色谱扫描法同时检测豆制品中碱性橙、皂黄、柠檬黄和日落黄以及辣椒粉中酸性橙Ⅱ、丽春红2R和罗丹明B[J].分析试验室,2010,29(6):15-18.Xia LY,Han YY,Kuang LH,et al.Simultaneous determination of basic orangeⅡ,metanil yellow,tartrazine,sunset yellow in bean-product and acid orangeⅡ,ponceau 2R,rhodanmine B in chili powder by thin-layer chromatographic scanning[J].Chin J Anal Lab,2010,29(6):15-18.
[17]吴彦蕾,林晓洋,胡靖,等.高效液相色谱法快速检测食品中18种合成色素[J].食品工业科技,2013,34(24):49-52.Wu YL,Lin XY,Hu J,et al.Fast determination of 18 synthetic colors in foods by high performance liquid chromatography[J].Sci Technol Food Ind,2013,34(24):49-52.
[18]刘杰,王占利,张先聚,等.果汁果酱与乳制品中苯甲酸、山梨酸同步检测实验[J].中国奶牛,2014,(19):29-31.Liu J,Wang ZL,Zhang XJ,et al.Simultaneous determination of benzoic acid and sorbic acid in fruit juice and jam and dairy products[J].China Dairy Cattle,2014,(19):29-31.
[19]GB/T 27404-2008实验室质量控制规范食品理化检测[S].GB/T 27404-2008 Criterion on quality control of laboratories-Chemical testing of food[S].
[20]赵灵芝,刘春叶,王海洋,等.高效液相色谱法测定硝苯地平片含量的方法学研究[J].化学与生物工程,2014,31(07):70-72.Zhao LZ,Liu CY,Wang HY,et al.The methodological study for HPLCdetermination of nifedipine content[J].Chem Bioeng,2014,31(7):70-72.
[21]崔连喜,张肇元,吴宇峰,等.样品溶剂对高效液相色谱分析结果的影响[J].广州化工,2016,44(18):157-158.Cui LX,Zhang ZY,Wu YF,et al.Effect of sample solvent on HPLCanalysis results[J].Guangzhou Chem Ind,2016,44(18):157-158.