高效液相色谱-串联质谱法测定保健食品中的番茄红素

食品科学 ›› 2012, Vol. 33 ›› Issue (20): 206-211.

高效液相色谱-串联质谱法测定保健食品中的番茄红素

陈冬东1,2，郗存显3，彭涛2，王俊苏3，张雷3，李贤良3，李应国3，

1.中国农业大学理学院 2.中国检验检疫科学研究院 3.重庆出入境检验检疫局，重庆市进出口食品安全工程技术研究中心

收稿日期:2011-08-11 修回日期:2012-09-19 出版日期:2012-10-25 发布日期:2012-11-09
通讯作者: 陈冬东 E-mail:cdd2240_1@126.com
基金资助:
国家科技部十一五科技支撑项目

Determination of Lycopene in Dietary Supplements by High Performance Liquid Chromatography-Tandem Mass Spectrometry

Received:2011-08-11 Revised:2012-09-19 Online:2012-10-25 Published:2012-11-09
Contact: CHEN Dong-Dong E-mail:cdd2240_1@126.com

摘要/Abstract

摘要： 建立保健食品中番茄红素的液相色谱-串联质谱测定方法。样品经氢氧化钾溶液乙醇皂化，去除脂肪后用质量浓度为1g/100mL的2,6-二叔丁基-4-甲基苯酚(BHT)石油醚溶液提取，提取液经中性氧化铝固相萃取柱净化，采用液相色谱-质谱联用技术-大气压化学电离源多反应监测模式检测，外标法定量。方法的检出限和定量限分别为10μg/kg和100μg/kg，在50～5000μg/kg添加水平范围内，平均回收率为88.0%～103.1%，相对标准偏差低于15%。本方法灵敏，为保健食品中番茄红素的定量检测和确证提供了新的手段。

关键词: 番茄红素, 保健食品, 测定, 液相色谱-串联质谱法

Abstract: A comprehensive analytical method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of lycopene in dietary supplements. Samples were saponified to remove lipid, followed by vortex-assisted extraction with petroleum ether containing 1 g/100 mL 2,6-di-tert-butyl-4-methylphenol (BHT). The resulting extract was further cleaned up on a neutral alumina solid-phase extraction cartridge. The pooled eluate was determined on LC-MS/MS by atmospheric pressure chemical ionization coupled with a multiple reaction-monitoring (MRM) mode. Lycopene was quantified by external standard method. The limit of detection (LOD) was 10 μg/kg, and the limit of quantification (LOQ) was 100 μg/kg. The average recovery rates of lycopene across six spike levels, 50.0, 100.0, 250.0, 500.0, 2500.0 μg/kg and 5000.0 μg/kg were 88.0%–103.1% with a relative standard deviation less than 15% (n=6). This method is sensitive and provides a new approach for the quantitative analysis and validation of lycopene in dietary supplements.

Key words: lycopene, dietary supplements, determination, liquid chromatography-tandem mass spectrometry

中图分类号:

陈冬东1,2，郗存显3，彭?涛2，王俊苏3，张?雷3，李贤良3，李应国3，. 高效液相色谱-串联质谱法测定保健食品中的番茄红素[J]. 食品科学, 2012, 33(20): 206-211.

参考文献

参考文献
[1] 杨万政,常华,杜晓鸣. 番茄红素的稳定性研究[J].内蒙古医学院学报, 2009, 31(3): 176-180.
[2] Lime B. J., Griffiths F. P., O’Connor R. T., et al. Grapefruit Pigment Determination, Spectrophotometric Methods for Determining Pigmentation-Beta-Carotene and Lycopene-in Ruby Red Grapefruit[J]. J. Agric. Food Chem., 1957, 5(12): 941-944.
[3] Johjima Tomio, Oguar Hiroshi. Analysis of Tomato Carotenoids by Thin-Layer Chromatography and a Cis-form γ-Carotene Newly Identified in Tangerine Tomato[J].J. Japan. Soc. Hort. sci., 1983, 52(2): 200-209.
[4] Olives Barba A.I., Cámara Hurtado M., Sánchez Mata M.C., Fernández Ruiz V., López Sáenz de Tejada M.. Application of a UV–vis detection-HPLC method for a rapid determination of lycopene and β-carotene in vegetables[J]. Food Chem., 2006, 95(2): 328-336.
[5] Tzouganaki Z. D., Atta-Politou J., Koupparis M. A.. Development and validation of liquid chromatographic method for the determination of lycopene in plasma[J]. Anal. Chim. Acta, 2002, 467(1-2): 115-123.
[6] Kenneth W. Miller, Nancy A. Lorr and Chung S. Yang. Anal. Biochem. Simultaneous determination of plasma retinol, α-tocopherol, lycopene, α-carotene, and β-carotene by high-performance liquid chromatography[J], Anal. Biochem.,1984, 138(2): 340-345.
[7] M.V. Vertzoni, C. Reppas, H.A. Archontaki. Optimized determination of lycopene in canine plasma using reversed-phase high-performance liquid chromatography[J],J. Chromatogr. B, 2005, 819(1): 149-154.
[8] Xu F., Yuan Q.P., Dong H.R.. Determination of lycopene and β-carotene by high-performance liquid chromatography using sudan I as internal standard[J]. J. Chromatogr. B, 2006, 838(1): 44-49.
[9] Froescheis O., Moalli S., Liechti H., Bausch J.. Determination of lycopene in tissues and plasma of rats by normal-phase high-performance liquid chromatography with photometric detection[J]. J. Chromatogr. B, 2000, 793(2): 291-299.
[10] Jaroslav Pól,Tuulia Hy?tyl?inen, Outi Ranta-Aho,Marja-Liisa Riekkola. Determination of lycopene in food by on-line SFE coupled to HPLC using a single monolithic column for trapping and separation[J]. J. Chromatogr. A, 2004, 1052(1-2): 25-31.
[11] Broich Carla R., Erdman Leonard E. Gerber. John W.. Determination of lycopene, α- and β-carotene and retinyl esters in human serum by reversed-phase high performance liquid chromatography[J]. Lipids,1983, 18(3): 253-258.
[12] Hagiwara Teruhiko, Yasuno Tetsuko, Funayama Keiichi, Suzuki Sukeji. Determination of lycopene, α-carotene and β-carotene in serum by liquid chromatography–atmospheric pressure chemical ionization mass spectrometry with selected-ion monitoring[J]. J. Chromatogr. B, 1998, 708(1-2): 67-73.
[13] Richard B. van Breemen, Xu Xiaoying, Viana Marlos A., Chen Longwen, Maria Stacewicz-Sapuntzakis, Duncan Claudine, Bowen Phyllis E., Sharifi Roohollah . Liquid Chromatography?Mass Spectrometry of cis- and all-trans-Lycopene in Human Serum and Prostate Tissue after Dietary Supplementation with Tomato Sauce[J]. J. Agric. Food Chem., 2002, 50(8): 2214-2219.
[14] Fang Liqiong, Pajkovic Natasa, Wang Yan, Gu Chungang, Richard B. van Breemen. Quantitative Analysis of Lycopene Isomers in Human Plasma Using High-Performance Liquid Chromatography?Tandem Mass Spectrometry[J]. Anal. Chem., 2003, 75(4): 812-817.
[15]张军,杜平,孙立霞. 快速高分离度液相色谱-串联质谱法测定番茄酱中番茄红素的含量[J].中国食物与营养, 2010, 6: 54-56.
[16]王超,张昭. 番茄红素的提取与稳定性研究[J].江苏科技大学学报(自然科学版)，2010，24(2): 188-192.
[17] 张丽薇,崔勇,李青. 高效液相色谱法测定保健食品中的番茄红素[J].中国卫生检验杂志, 2008, 18(6): 1069-1070.
[18] Jannat M. Roldán-Gutiérrez, María Dolores Luque de Castro. Trac Trend. Lycopene: The need for better methods for characterization and determination[J]. Anal. Chem., 2007, 26(2): 163-170.
[19] Zuehlke, S.; Duennbier, U.; Heberer, T. Determination of Polar Drug Residues in Sewage and Surface Water Applying Liquid Chromatography?Tandem Mass Spectrometry[J]. Anal. Chem., 2004, 76(22): 6548-6554.
[20] Vanderford, B. J., Pearson, R. A., Rexing, D. J. Analysis of Endocrine Disruptors, Pharmaceuticals, and Personal Care Products in Water Using Liquid Chromatography/Tandem Mass Spectrometry[J]. Anal. Chem., 2003, 75 (22):6265–6274.
[20] Matuszewski, B. K.; Constanzer, M. L.; Chavez-Eng, C. M. Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS. Anal. Chem. , 2003, 75: 3019-3030.