全自动固相萃取-液相色谱法同时测定饮料中的11种合成着色剂-食品安全质量检测学报-CSCIED科技核心评价数据库-手机版

全自动固相萃取-液相色谱法同时测定饮料中的11种合成着色剂

Simultaneous determination of 11 kinds of synthetic colorants in beverages by automated solid-phase extraction-liquid chromatography

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DOI	10.19812/j.cnki.jfsq11-5956/ts.20250212005
刊名	食品安全质量检测学报 Journal of Food Safety and Quality
年，卷(期)	2025, 16(13)
作者	李彪, 张岩岩, 徐宏岩*,
作者单位	阜阳市产品质量监督检验所; 国家再生有色金属橡塑材料质量监督检验中心(安徽)
摘要	目的建立全自动固相萃取-液相色谱法同时测定饮料中11种合成作色剂含量的方法。方法取2 g饮料试样, 用氨水乙醇溶液提取, 借助全自动固相萃取仪依次进行活化、上样、淋洗、洗脱、收集操作, 氮吹复溶后采用液相色谱仪[二极管阵列多波长多通道同时检测, 检测波长 415 nm(柠檬黄、喹啉黄), 520 nm(新红、苋菜红、胭脂红、日落黄、诱惑红、酸性红和赤藓红), 610 nm(靛蓝、亮蓝); 流动相: A为20 mmol/L乙酸铵溶液, B为甲醇, 流速1 mL/min梯度洗脱]上机测定。结果在0.2~10.0 μg/mL质量浓度范围内, 11种合成着色剂的浓度与峰面积呈现良好线性关系, 线性相关系数均大于0.99, 检出限符合GB 5009.35—2023《食品安全国家标准食品中合成作色剂的测定》要求。标准加入法回收试验中, 回收率处于91.3%~106.0%, 测定值的相对标准偏差(n=6)均小于5.0%。将该方法应用于长三角食品类检测机构饮料中的胭脂红、日落黄能力验证, 胭脂红含量为5.86 mg/kg, 日落黄含量为4.31 mg/kg, 其余合成着色剂均未检出。结论该方法前处理富集效果好、自动化程度高、操作简单、稳定性好、时间短、效率高、灵敏性好, 准确度高、重现性好, 适用于大批量饮料中合成着色剂的测定分析。
Abstract	Objective To establish a method for the simultaneous determination of 11 kinds of synthetic colorants in beverages by automated solid-phase extraction-liquid chromatography. Methods The 2 g of the beverage sample was taken, it was extracted with an ammonia ethanol solution, and operations such as activation, sample loading, washing, eluting and collection were performed in turn with the help of a fully automatic solid-phase extraction instrument. After nitrogen blowing and redissolution, the liquid chromatography instrument was used for on-line determination [diode multi-wavelength multi-channel simultaneous detection, detection wavelengths 415 nm (citrus yellow and quinoline yellow), 520 nm (new red, amaranth red, carmine, sunset yellow, temptation red, acidic red, and red algae), 610 nm (indigo and bright blue); mobile phase: A 20 mmol/L ammonium acetate solution, B methanol, flow rate 1 mL/min, gradient elution]. Results In the range of 0.2–10.0 μg/mL, the mass concentration of 11 kinds of synthetic colorants showed good linear relationship with peak area, and the linear correlation coefficients were all greater than 0.99, the limit of detection met the requirements of GB 500935—2023 National food safety standard-Determination of synthetic colorants in food. In the standard addition method recovery test, the recovery rates were between 91.3% and 106.0%, and the relative standard deviation of the determination value (n=6) was less than 5.0%. This method was applied to the ability verification of sunset yellow and carmine in beverages in food testing institutions in the Yangtze River Delta. The content of carmine was 5.86 mg/kg, and the content of sunset yellow was 4.31 mg/kg. The other synthetic colorants were not detected. Conclusion This method achieve good enrichment effect, high automation degree, simple operation, good stability, short time, high efficiency, good sensitivity, high accuracy and good reproducibility, and is suitable the determination and analysis of synthetic colorants in a large number of beverages.
关键词	全自动固相萃取法；高效液相色谱法；合成着色剂；饮料
KeyWord	automatic solid-phase extraction; liquid chromatography; synthetic colorant; beverage
基金项目
页码	155-161

参考文献
相关文献

[1]谢赛. 料中合成着色剂的研究进展
[J]. 现代食品, 2021, 17: 11–22. XIE S. Research progress on synthetic colorants in beverages
[J]. Modern Food, 2021, 17: 11–22.
[2]CHEN YF, SUN YF, PANG XM, et al. Three-dimensional dual-network magnetic conductive hydrogel for the highly sensitive electrochemical detection of ponceau 4R in foods
[J]. Biosensors and Bioelectronics, 2023, 241: 115698.
[3]何林. 几种食品添加剂的遗传毒性及其联合毒性研究
[D]. 广州: 暨南大学, 2008. HE L. Research on the genotoxicity and combined toxicity of several food additives
[D]. Guangzhou: Ji’nan University, 2008.
[4]曾盈, 蔡智鸣, 王振, 等. 胭脂红对3T3细胞DNA损伤的SCGE检测
[J]. 同济大学学报(医学版), 2008, 29(1): 41–44. ZENG Y, CAI ZM, WANG Z, et al. SCGE detection of DNA damage in 3T3 cells by carmine
[J]. Journal of Tongji University (Medical Science Edition), 2008, 29(1): 41–44.
[5]马晓燕. 几种合成色素的同时检测及其对细胞毒性研究
[D]. 北京: 中国计量大学, 2012. MA XY. Simultaneous detection of several synthetic dyes and their study on cytotoxicity
[D]. Beijing: China University of Metrology, 2012.
[6]陈玉银, 杜鑫, 靳远祥. 食用色素对家蚕毒性的试验
[J]. 蚕桑通报, 2005, 36(3): 27–34. CHEN YY, DU X, JIN YX. Experimental study on the toxicity of food dyes to the silkworm
[J]. Bulletin of Sericulture, 2005, 36(3): 27–34.
[7]COMBES R, HAVELAND S. A review of the genotoxicity of food, drug and cosmetic colours and other azo, triphenylmethane and xanthene dyes
[J]. Mutation Research, 1982, 98: 101–243.
[8]丁成翔, 代汉慧, 陈冬东. 六种着色剂毒性研究进展
[J]. 检验检疫学刊, 2009, 19: 70–73. DING CX, DAI HH, CHEN DD. Research progress on the toxicity of six colorants
[J]. Quality Safety Inspection and Testing, 2009, 19: 70–73.
[9]李家玉, 王海滨, 林志华, 等. 合成色素的危害及其分析方法
[J]. 中国园艺文摘, 2009, 25(10): 165–167. LI JY, WANG HB, LIN ZH, et al. Hazards of synthetic pigments and their analysis methods
[J]. Chinese Horticulture Abstracts, 2009, 25(10): 165–167.
[10]张晓文, 钟鑫, 易文珂. 食用色素的应用及其危害
[J]. 化工管理, 2014(27): 31. ZHANG XW, ZHONG X, YI WK. Application and hazards of food pigments
[J]. Chemical Engineering Management, 214(27): 31.
[11]周宇, 王彦钧, 郑乔方, 等. 儿童软糖中合成着色剂的含量测定及健康风险评估
[J]. 食品安全质量检测学报, 2024, 15(13): 186–192. ZHOU Y, WANG YJ, ZHENG QF, et al. Determination of synthetic colorants content in children’s gummy bears health risk assessment
[J]. Journal of Food Safety & Quality, 2024, 15(13): 186–192.
[12]新疆维吾尔自治区市场监督管理局. 新疆维吾尔自治区市场监督管理局食品安全监督抽检信息通告(2020年第19期)2020年第57号
[EB/OL]. (2020-07-10)
[2025-04-07]. https://scjgj.xinjiang.gov.cn/xjaic/tzgg/ 202007/553c738c4fc849fa8f81840544496a6f.shtml Xinjiang Uygur Autonomous Region Market Supervision. Xinjiang Uygur Autonomous Region Market Supervision bureau announcement of food safety supervision and spot inspection information (No.19 of 2020) 2020 No.57
[EB/OL]. (2020-07-10)
[2025-04-07]. https://scjgj.xinjiang.gov.cn/ xjaic/tzgg/202007/553c738c4fc849fa8f81840544496a6f.shtml
[13]广州市市场监督管理局. 广州市市场监督管理局2021年第25期食品安全监督抽检信息(自制饮品专项)
[EB/OL]. (2021-08-26)
[2025-04-07]. https://www.gz.gov.cn/zwgk/zdly/spypaq/zlxx/spzlxx/content/post_7742174.html Guangzhou Municipal Market Supervision Bureau. Guangzhou Municipal Market Supervision Bureau, 2021 No.25 safety supervision and inspection information (homemade beverage special)
[EB/OL]. (2021-08-26)
[2025-04-07]. https://www.gz.gov.cn/zwgk/zdly/spypaq/zlxx/spzlxx/ content/ post_7742174.html
[14]贵州省市场监管局食品安全抽检监测处. 贵州省市场监管局关于22批次食品抽检不合格情况的通告(2023年第17期)
[EB/OL]. (2023-06-08)
[2025-04-07]. https://www.guizhou.gov.cn/zwgk/zdlygk/qlyxjggjg/spaq/ spcj/202306/t20230608_80121056.html Food Safety Inspection and Monitoring Department of Guizhou Provincial Market Supervision Administration. Guizhou Provincial Market Supervision Administration announcement the inspection of 22 batches of unsafe food (issue 17, 2023)
[EB/OL]. (2023-06-08)
[2025-04-07]. https://www.guizhou.gov.cn/zwgk/zdlygk/qlyxjggjg/spaq/spcj/202306/t20230608_80121056.html
[15]河南省市场监督管理局(知识产权局). 河南省市场监督管理局关于20批次食品不合格情况的通告(2023年第21期)
[EB/OL]. (2023-06-14)
[2025-04-07]. https://scjg.henan.gov.cn/2023/06-14/2760822.html Henan Provincial Market Supervision (Intellectual Property Bureau). Announcement on the unqualified status of 20 batches of food by the Henan Provincial Market Supervision (issue 21, 2023)
[EB/OL]. (2023-06-14)
[2025-04-07]. https://scjg.henan.gov.cn/2023/06-14/2760822. html
[16]湖北省市场监督管理局. 湖北省市场监督管理局食品安全监督抽检信息公告(2024年第5期)
[EB/OL]. (2024-05-29)
[2025-04-07]. http://scjg.hubei.gov.cn/zfxxgk/fdzdgknr/zdly/spjg/cjgg/202405/t20240529_5219777.shtml Hubei Provincial Market Supervision Bureau. Announcement of food safety supervision and spot inspection information of Hubei Provincial Market Supervision and Administration Bureau (issue 5, 2024)
[EB/OL]. (2024-05-29)
[2025-04-07]. http://scjg.hubei.gov.cn/zfxxgk/fdzdgknr/ zdly/spjg/cjgg/202405/t20240529_5219777.shtml
[17]王婷, 程国栋, 李娜, 等. 高效液相色谱法同时测定食品中9种合成着色剂
[J]. 食品安全质量检测学报, 2022, 13(2): 483–491. WANG T, CHENG GD, LI N, et al. Simultaneous determination of 9 kinds of synthetic colorants in foods by high performance liquid chromatography
[J]. Journal of Food Safety & Quality, 2022, 13(2): 483–491.
[18]HU X, LI W, ZHANG Y. Development of a rapid screening method for synthetic colorants in food using spectroscopy techniques
[J]. Talanta, 2023, 254: 123456–123463.
[19]LI N, ZHAO X, CHEN Y. Evaluation of the performance of solid-phase extraction columns for synthetic colorants
[J]. Journal of Separation Science, 2022, 45(15): 3214–3221.
[20]陈小华. 固相萃取技术与应用
[M]. 第二版. 北京: 科学出版社, 2019. CHEN XH. Solid-phase extraction technology and its applications
[M]. Second Edition. Beijing: Science Press, 2019.
[21]LIU M, WANG S, ZHANG H. Study on the detection limits and accuracy of synthetic colorant analysis methods
[J]. Journal of AOAC International, 2023, 106(3): 678–685.
[22]CHEN W, WANG X, ZHANG Y. Application of solid-phase microextraction in the analysis of synthetic colorants in beverages
[J]. Journal of Agricultural and Food Chemistry, 2022, 70(34): 10987–10994.
[23]LI F, LIU X, ZHANG M. Optimization of chromatographic conditions for the separation of multiple synthetic colorants
[J]. Journal of Chromatography A, 2021, 1647: 456–463.
[24]LIU G, LI Y, ZHAO J. Comparison of different detectors for the determination of synthetic colorants in food
[J]. Analytical Letters, 2020, 53(18): 2897–2904.
[25]YANG J, CHEN Q, LIU H. Influence of pH on the extraction efficiency of synthetic colorants in beverages
[J]. Food Research International, 2022, 158: 111345–111352.
[26]CHEN H, LI M, ZHAO J. Optimization of sample preparation for the analysis of synthetic colorants in beverages
[J]. Journal of Chromatography B, 2023, 1234: 123–130.
[27]ZHANG X, LIU Z, WANG Q. Comparison of different extraction solvents for synthetic colorants in food products
[J]. Journal of Agricultural and Food Chemistry, 2020, 68(45): 12345–12352.
[28]LIU Y, WANG X, ZHANG Y. Simultaneous determination of multiple synthetic colorants in food by liquid chromatography-tandem mass spectrometry
[J]. Food Chemistry, 2022, 384: 132456–132463.
[29]LI H, ZHAO X, LIU M. Study on the interference of coexisting substances in the determination of synthetic colorants
[J]. Journal of AOAC International, 2023, 106(5): 1123–1130.
[30]WANG Y, ZHAO N, CHEN X. Effect of sample matrix on the determination of synthetic colorants by liquid chromatography
[J]. Journal of Separation Science, 2020, 43(20): 3897–3904.
[31]赵鹏, 黄亚琴, 徐奋奋, 等. 固相萃取-高效液相色谱-可变波长检测法测定鲜榨果汁中7种水溶性合成着色剂
[J]. 中国卫生检验杂志, 2015, 25(8): 1159–1161, 1165. ZHAO P, HUANG YQ, XU FF, et al. Determination of 7 water-soluble synthetic colorants in freshly squeezed fruit juices by solid-phase extraction-high performance liquid chromatography-variable wavelength detection
[J]. Chinese Journal of Health Laboratory Technology, 2015, 25(8): 1159–1161, 1165.
[32]李晓芹, 徐振东. 固相萃取-高效液相色谱法在食品中合成着色剂检测中的应用
[J]. 食品工业, 2014, 35(6): 56–58. LI XQ, XU ZD. Application of solid-phase extraction-high performance liquid chromatography in the detection of synthetic colorants in foods
[J]. The Food Industry, 2014, 35(6): 56–58.
[33]汪强, 黄宇, 张月松, 等. 固相萃取-高效液相色谱-二极管阵列检测法测定饮料中9种人工合成着色剂
[J]. 食品安全导刊, 2021(10): 50–54. WANG Q, HUANG Y, ZHANG YS, et al. Determination of 9 artificial synthetic colorants in beverages by solid-phase extraction-high performance liquid chromatography-diode array detection
[J]. China Food Safety Magazine, 2021(10): 50–54.
[34]李彤辉, 尚伟, 周楠, 等. 固相萃取-高效液相色谱法检测多种食品基质中10种合成着色剂方法研究
[J]. 现代食品科技, 2019, 35(2): 279–284. LI TH, SHANG W, ZHOU N, et al. Study on the method of detecting 10 synthetic colorants in multiple food matrices by solid-phase extraction-high performance liquid chromatography
[J]. Modern Food Science and Technology, 2019, 35(2): 279–284.

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李彪, 张岩岩, 徐宏岩*. 全自动固相萃取-液相色谱法同时测定饮料中的11种合成着色剂 [J]. 食品安全质量检测学报. 2025; 16; (13). 155 - 161.

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