乙酸酐衍生GC-ECD法测定饮料中三氯蔗糖含量

doi:10.7506/spkx1002-6630-201614037

摘要/Abstract

摘要：

建立一种乙酸酐衍生-气相色谱-电子捕获器检测食品中三氯蔗糖含量的方法。样品经水稀释、1-甲基咪唑催化、乙酸酐衍生，生成的衍生物采用气相色谱-质谱法定性，气相色谱-电子捕获器法定量。结果表明：衍生目标物为4,1’,6’-三氯-2,3,6,3’,4’-五乙酰基蔗糖，并且在0.02～1.2 mg/mL范围内线性关系良好（R= 0.999 4），检出限为0.23 mg/kg，回收率为90.0%～94.5%，相对标准偏差（n=6）为0.6%～2.5%。该方法操作简单、干扰少、检出限低、灵敏度高、线性好、结果准确，能很好地满足饮料中三氯蔗糖含量的测定。

关键词: 三氯蔗糖, 乙酸酐衍生, 气相色谱-电子捕获器, 气相色谱-质谱联用

Abstract:

A gas chromatographic (GC) method with an electron capture detector (ECD) after acetylation was developed
for the determination of sucralose in drinks. Samples were diluted with water and then derivatized with acetic anhydride
in the presence of 1-methylimidazole as a catalyst. Qualitative and quantitative analyses of the derivatives were achieved
by GC-MS and GC-ECD, respectively. The results showed that the target derivative was 4,1’,6’-trichloro-2,3,6,3’,4’-
sucrose pentaacetate (TOSPA). The calibration curve for the analyte showed good linearity in the range of 0.02–1.2 mg/mL
(R = 0.999 4). The limit of detection (LOD) for sucralose was 0.23 mg/kg, and the recoveries obtained by standard addition
method were between 90.0% and 94.5%, with relative standard deviations (RSD, n = 6) between 0.6% and 2.5%. This
method provides the advantages of low LOD, high sensitivity, less disturbance, good linearity, high accuracy and simple
operation. Thus, it can be applied in sucralose analysis in drinks.

Key words: sucralose, derivatization with acetic anhydride, gas chromatography-electron capture detector (GC-ECD), gas chromatography-mass spectrometry (GC-MS)

中图分类号:

O657

黄志勇，陈艳，冯慧，刘超，景赞. 乙酸酐衍生GC-ECD法测定饮料中三氯蔗糖含量[J]. 食品科学, doi: 10.7506/spkx1002-6630-201614037.

HUANG Zhiyong, CHEN Yan, FENG Hui, LIU Chao, JING Zan. Determination of Sucralose in Drinks by Gas Chromatography with Electron Capture Detector (GC-ECD) after Derivatization with Acetic Anhydride[J]. FOOD SCIENCE, doi: 10.7506/spkx1002-6630-201614037.

参考文献

[1] 凌关庭. 食品添加剂手册[M]. 3版. 北京: 化学工业出版社, 2003:

160-161.

[2] 张玉, 吴慧明, 徐丽红, 等. 三氯蔗糖的安全性研究进展[J]. 食品工

业科技, 2011, 32(11): 472-474.

[3] 高金燕, 陈红兵. 三氯蔗糖在无糖巧克力和口香糖中的应用[J]. 食

品工业, 2004, 25(5): 5-6.

[4] KNIGHT I. The development and applications of sucralose: a new

high-intensity sweetener[J]. Canadian Journal of Physiology and

Pharmacology, 1994, 72(4): 435-439. DOI:10.1139/y94-063.

[5] 周力. 三氯蔗糖的生产与应用[J]. 食品科学, 1997, 18(8): 38-41.

[6] 胡莉蓉. 新型甜味剂三氯蔗糖[J]. 化工时刊, 2005, 19(3): 50-55.

[7] BIGAL M E, KRYMCHANTOWSKI A V. Migraine triggered

by sucralose-a case report[J]. Headache, 2006, 46(3): 515-517.

DOI:10.1111/j.1526-4610.2007.00735.x·2.71.

[8] SUEZ J, KOREM T, ZEEVI D, et al. Artificial sweeteners induce

glucose intolerance by altering the gut microbiota[J]. Nature, 2014,

514: 181-186. DOI:10.1038/nature13793.

[9] 卫生部. GB 2760—2014 食品添加剂使用标准[S]. 北京: 中国标准

出版社, 2014.

[10] 倪炜华, 郑丹. LC-MS法测定饮料中的三氯蔗糖[J]. 中国食品添加

剂, 2011(2): 235-238. DOI:10.3969/j.issn.1006-2513.2011.02.037.

[11] 周莉莉, 杨颖, 刘艳明, 等. 超高效液相色谱-串联质谱法测定

食品中的三氯蔗糖[J]. 分析测试学报, 2011, 30(10): 1175-1178.

DOI:10.3969/j.issn.1004-4957.2011.10.019.

[12] KOYAMA M, YOSHIDA K, UCHIBORI N, et al. Analysis of nine

kinds of sweeteners in foods by LC/MS[J]. Shokuhin Eiseigaku

Zasshi, 2005, 46(3): 72-78. DOI:10.1016/j.jfda.2014.01.0240.62.

[13] NOJIRI S, NAKAZATO M, KASUYA Y, et al. Determination of

sucra-lose in foods by HPLC using pre-column derivatization[J].

Shokuhin Eiseigaku Zasshi, 2002, 43(5): 289-294.

[14] 陈璐莹, 刘亚攀, 冉雪琴, 等. 紫外衍生-高效液相色谱法测定保健

食品和饮料中的三氯蔗糖[J]. 四川大学学报(医学版), 2014, 45(5):

836-838. DOI:10.13464/j.scuxbyxb.2014.05.023.

[15] 张莉. 高效液相色谱法测定饮料中三氯蔗糖的含量[J]. 中国卫生检

验杂志, 2007, 17(10): 1784-1786.

[16] 张伟清, 张玉婷, 曹进, 等. 酱油及酱制品中三氯蔗糖的测定[J].

食品科学, 2013, 28(20): 237-240. DOI:10.7506/spkx1002-6630-

2013180050.

[17] 熊丽蓓, 戴承兵, 何倩琼. 高效液相色谱法测定食品中三氯蔗糖含

量的研究[J]. 上海预防医学杂志, 2005, 17(4): 156-158.

[18] 粟晖, 韦异, 张英, 等. 反相高效液相色谱法分离测定三氯蔗糖[J].

食品工业科技, 2002, 23(6): 66-67.

[19] 卫生部. GB/T 22255—2014 食品中三氯蔗糖(蔗糖素)的测定[S]. 北

京: 中国标准出版社, 2014.

[20] 周维义, 邓小娟. 高效液相色谱法分析三氯蔗糖的含量[J]. 食品科

学, 2007, 28(7): 360-361.

[21] 陈晓霞, 游景水, 杨祖伟. 高效液相色谱法测定保健食品中三氯蔗

糖的含量[J]. 食品安全质量检测学报, 2015, 6(5): 1883-1888.

[22] QIU Wenlon, WANG Zhongfu, NIE Wanli, et al. GC-MS

determination of sucralose in splenda[J]. Chromatographia, 2007,

66(11): 935-939. DOI:10.1365/s10337-007-0422-4.

[23] FARHADI A, KESHAVARZIAN A, HOLMES E W, et al.

Gas chromatographic method for detection of urinary sucralose:

application to the assessment of intestinal permeability[J]. Journal

of Chromatography B, 2003, 784: 145-154. DOI:10.1016/S0002-

9270(02)04713-5.

[24] 廖洪梅, 戴玲, 魏晓飞, 等. 单糖乙酰化条件的优化[J]. 理化检验(化

学分册), 2008, 44(5): 441-443.

[25] 贺永惠, 王清华, 刘长忠, 等. 乙酸酐衍生化气相色谱法测定小麦非

淀粉多糖的单糖组成[J]. 光谱实验室, 2009, 26(4): 1040-1042.