HPLC Determination of Vanillin and Ethyl Vanillin in Cosmetics
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摘 要
对膏状样品取1.0 g,加入四氢呋喃4 mL溶解后用甲醇定容至10 mL;对乳状、水状及固体样品取1.0 g,加入甲醇至近5 mL,涡旋振荡1 min,用甲醇定容至10 mL。将上述试样溶液超声提取15 min,离心分层,取上清液,用ZORBAX Eclipse Plus C18色谱柱为分离柱,以甲醇与1.5%(体积分数)乙酸溶液按体积比35:65组成的混合液为流动相,作色谱分离,在波长280 nm处进行紫外检测。测得香兰素和乙基香兰素的质量浓度均在0.5~100 mg·L-1内与其对应的峰面积呈线性关系,其检出限(3S/N)均为0.2 mg·kg-1。以空白样品为基体,用标准加入法进行回收试验,测得回收率为91.3%~97.0%,测定值的相对标准偏差(n=6)为1.0%~1.7%。
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Abstract
For creamy sample, 1.0 g was taken and dissolved in 4 mL of tetrahydrofuran, and then its volume was made up to 10 mL with methanol. For emulsion, aqueous or solid sample, 1.0 g was taken and methanol was added to make its total volume to near 5 mL, the mixture was shaked for 1 min by swirling. The total volume was then made up to 10 mL with methanol. For either case, the sample solution was extracted ultrasonically for 15 min, and centrifuged for phase separation. The supernatant was taken and chromatographic separation was made by using ZORBAX Eclipse Plus C18 column as the separation column and mixture composed of methanol and 1.5% (φ) acetic acid solution (mixed in the volumic ratio of 35 to 65) as the mobile phase. UV-detection at 280 nm was adopted. Linear relationships between values of peak area and mass concentration of vanillin and ethyl vanillin were found in the same range of 0.5-100 mg·L-1, with same detection limits (3S/N) of 0.2 mg·kg-1. Test for recovery was made by standard addition method using a blank sample as matrix, values of recovery found were ranged from 91.3% to 97.0%. Values of RSD (n=6) found were in the range of 1.0%-1.7%.
中图分类号 O652.63 DOI 10.11973/lhjy-hx201711016
所属栏目 工作简报
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收稿日期 2016/11/20
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备注黄键(1984-),男,江苏南通人,工程师,主要从事食品、化妆品安全的检测研究工作,huangj2@jsciq.gov.cn
引用该论文: HUANG Jian,ZHANG Wenguo,GUO Guiping,NI Peng,SHI Jinhui,WANG Jinjuan. HPLC Determination of Vanillin and Ethyl Vanillin in Cosmetics[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(11): 1318~1321
黄键,张文国,郭桂萍,倪鹏,施锦辉,王金娟. 高效液相色谱法同时测定化妆品中香兰素和乙基香兰素的含量[J]. 理化检验-化学分册, 2017, 53(11): 1318~1321
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参考文献
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【9】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, 2014,33(2):208-211.
【10】单秀梅,卢忠魁,黄越.反相高效液相色谱法测定啤酒中香兰素[J].中国卫生工程学, 2003,2(2):109-110.
【11】韩双,杨金宝,刘宁.气相色谱-质谱/选择离子法测定牛奶中的香兰素[J].中国乳品工业, 2008,36(8):53-55.
【12】林灵超,吴方圆.高效液相色谱法同时测定牛奶中的香兰素与乙基香兰素[J].化学分析计量, 2013,22(2):60-62.
【13】肖珊珊,孙兴权,李一尘,等.高效液相色谱法测定软饮料中香兰素和乙基香兰素[J].食品安全质量检测学报, 2015,6(1):152-158.
【14】单之初,俞红波,沈翔,等.气相色谱法测定黄酒中香兰素含量[J].酿酒科技, 2015(9):125-127.
【15】倪永年,姜云娜.线性扫描溶出伏安法测定食品中的乙基香兰素[J].南昌大学学报(理科版), 2005,29(3):269-271.
【16】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 Chem, 2005,89(3):465-473.
【17】LUQUE M, LUQUE-PÉREZ E, RÍOS A, et al. Supported liquid membranes for the determination of vanillin in food samples with amperometric detection[J]. Anal Chim, 2000,410(1/2):127-134.
【18】张国文,倪永年.偏最小二乘-吸光光度法同时测定食用香料香兰素和乙基香兰素[J].南昌大学学报(理科版), 2003,27(4):341-344.
【19】YARDIM Y, GVLCAN M, SENTVRK Z. Determination of vanillin in commercial food product by adsorptive stripping voltammetry using a boron-doped diamond electrode[J]. Food Chem, 2013,141(3):1821-1827.
【20】王建华.高效液相色谱法检测食品中香兰素的方法研究[J].中国卫生检验杂志, 2001,11(2):164-164.
【21】黄越,卢忠魁,卢刚.反相高效液相色谱法测定巧克力中香兰素[J].中国卫生检验杂志, 2002,12(5):566-566.
【22】周庆礼,黄艳凤,韩英素,等.高效液相色谱法测定发酵液中的香兰素[J].色谱, 2004,22(3):295-295.
【23】刘祥萍,黄薇.高效液相色谱法同时测定食品中的甲基香兰素和乙基香兰素[J].中华预防医学杂志, 2006,40(4):296-297.
【24】景丽洁,韩伟,闫光烈.用反相高效液相色谱法测定香兰素含量[J].食品科学, 2006,27(4):205-207.
【25】金海涛,马健瑜,王晓珣,等.高效液相色谱法同时测定香兰素与邻位香兰素[J].分析测试学报, 2011,30(2):222-224.
【26】宁霄,金绍明,曹进,等.高效液相色谱法测定乳制品中香兰素的含量[J].中国药师, 2015,18(2):312-315.
【2】刘玉萍.婴幼儿乳制品中香兰素的检测方法研究[J].湖南文理学院学报(自然科学版), 2011,23(2):51-54.
【3】欧菊芳,顾秀英,鲍忠定,等.气相色谱法测定婴幼儿配方奶粉中香兰素和乙基香兰素[J].江西科学, 2011,29(1):23-25.
【4】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.
【5】陶保华,储小军,赖世云,等.婴幼儿配方粉中香兰素和乙基香兰素的检测方法比较[J].食品安全质量检测学报, 2013,4(2):421-426.
【6】赵建国,姜金斗.气相色谱质谱联用测定婴幼儿奶粉中香兰素和乙基香兰素[J].生命科学仪器, 2013,11(5):40-44.
【7】肖锋,张毅,陈沛金,等.高效液相色谱-串联质谱法同时测定婴幼儿配方食品中香兰素、甲基香兰素和乙基香兰素[J].食品安全质量检测学报, 2014,5(11):3431-3436.
【8】黄晓林,宋戈.高效液相色谱法测定婴幼儿食品和乳品中香兰素及衍生物[J].中国乳品工业, 2014,42(4):57-58.
【9】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, 2014,33(2):208-211.
【10】单秀梅,卢忠魁,黄越.反相高效液相色谱法测定啤酒中香兰素[J].中国卫生工程学, 2003,2(2):109-110.
【11】韩双,杨金宝,刘宁.气相色谱-质谱/选择离子法测定牛奶中的香兰素[J].中国乳品工业, 2008,36(8):53-55.
【12】林灵超,吴方圆.高效液相色谱法同时测定牛奶中的香兰素与乙基香兰素[J].化学分析计量, 2013,22(2):60-62.
【13】肖珊珊,孙兴权,李一尘,等.高效液相色谱法测定软饮料中香兰素和乙基香兰素[J].食品安全质量检测学报, 2015,6(1):152-158.
【14】单之初,俞红波,沈翔,等.气相色谱法测定黄酒中香兰素含量[J].酿酒科技, 2015(9):125-127.
【15】倪永年,姜云娜.线性扫描溶出伏安法测定食品中的乙基香兰素[J].南昌大学学报(理科版), 2005,29(3):269-271.
【16】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 Chem, 2005,89(3):465-473.
【17】LUQUE M, LUQUE-PÉREZ E, RÍOS A, et al. Supported liquid membranes for the determination of vanillin in food samples with amperometric detection[J]. Anal Chim, 2000,410(1/2):127-134.
【18】张国文,倪永年.偏最小二乘-吸光光度法同时测定食用香料香兰素和乙基香兰素[J].南昌大学学报(理科版), 2003,27(4):341-344.
【19】YARDIM Y, GVLCAN M, SENTVRK Z. Determination of vanillin in commercial food product by adsorptive stripping voltammetry using a boron-doped diamond electrode[J]. Food Chem, 2013,141(3):1821-1827.
【20】王建华.高效液相色谱法检测食品中香兰素的方法研究[J].中国卫生检验杂志, 2001,11(2):164-164.
【21】黄越,卢忠魁,卢刚.反相高效液相色谱法测定巧克力中香兰素[J].中国卫生检验杂志, 2002,12(5):566-566.
【22】周庆礼,黄艳凤,韩英素,等.高效液相色谱法测定发酵液中的香兰素[J].色谱, 2004,22(3):295-295.
【23】刘祥萍,黄薇.高效液相色谱法同时测定食品中的甲基香兰素和乙基香兰素[J].中华预防医学杂志, 2006,40(4):296-297.
【24】景丽洁,韩伟,闫光烈.用反相高效液相色谱法测定香兰素含量[J].食品科学, 2006,27(4):205-207.
【25】金海涛,马健瑜,王晓珣,等.高效液相色谱法同时测定香兰素与邻位香兰素[J].分析测试学报, 2011,30(2):222-224.
【26】宁霄,金绍明,曹进,等.高效液相色谱法测定乳制品中香兰素的含量[J].中国药师, 2015,18(2):312-315.
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