分析与检测

超分子溶剂的制备及其在蚕蛹粉中黄曲霉毒素快速测定的应用

  • 王东旭 ,
  • 韦铮 ,
  • 王艳艳 ,
  • 杨帆 ,
  • 胡斯蒙
展开
  • (湖州市食品药品检验研究院,浙江 湖州,313000)
第一作者:博士,高级工程师(通信作者,E-mail:11237122@zju.edu.cn)

收稿日期: 2025-10-20

  修回日期: 2025-11-27

  网络出版日期: 2026-05-07

基金资助

湖州市公益性应用研究项目(2021GZ29)

Preparation and application of supramolecular solvents in determination of aflatoxins in silkworm pupae powder

  • WANG Dongxu ,
  • WEI Zheng ,
  • WANG Yanyan ,
  • YANG Fan ,
  • HU Simeng
Expand
  • (Huzhou Institute for Food and Drug Control, Huzhou 313000, China)

Received date: 2025-10-20

  Revised date: 2025-11-27

  Online published: 2026-05-07

摘要

基于蚕蛹粉中黄曲霉毒素污染引发的食品安全风险,该研究开发了一种盐析辅助超分子溶剂液液萃取结合超高效液相色谱-质谱同时检测蚕蛹粉中4种黄曲霉毒素高通量检测方法。通过对超分子溶剂比例、用量及盐析剂用量等关键因素进行考察优化,蚕蛹粉样本以正庚醇、四氢呋喃和水形成的超分子溶剂进行萃取,硫酸铵作为盐析助剂分层,提取液加水定容后,采用C18反相色谱柱分离,电喷雾正离子模式检测,外标法定量。最优实验条件下,在0.1~10.0 ng/mL范围内4种黄曲霉毒素线性良好,相关系数均大于等于0.999,检出限为0.03~0.12 μg/kg,定量限为0.1~0.4 μg/kg。3个浓度水平下加标回收率为77.3%~99.2%,精密度为0.4%~5.2%。该方法快捷、绿色、低廉,可满足对蚕蛹粉中4种黄曲霉毒素的快速准确分析要求。

本文引用格式

王东旭 , 韦铮 , 王艳艳 , 杨帆 , 胡斯蒙 . 超分子溶剂的制备及其在蚕蛹粉中黄曲霉毒素快速测定的应用[J]. 食品与发酵工业, 2026 , 52(8) : 396 -402 . DOI: 10.13995/j.cnki.11-1802/ts.044876

Abstract

Based on the food safety risks caused by aflatoxin contamination in silkworm pupa powder, a high-throughput detection method was developed using salting-out assisted supramolecular solvent liquid-liquid extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for simultaneous determination of four aflatoxins in silkworm pupa powder.After optimizing the key factors such as the composition and amount of supramolecular solvent,and the amount of salt,silkworm pupae powder samples were first subjected to extraction with a 1-heptanol/tetrahydrofuran/water-based supramolecular solvent, then salted out by sodium sulfate, separated on a C18 column, and finally determined by electrospray tandem mass spectrometry in positive ion and multiple reaction monitoring (MRM) mode, followed by external standard quantification.A strong linear response (r>0.999) was observed for all four aflatoxins across the tested range of 0.1 to 10.0 ng/mL.The established method provided detection and quantification limits of 0.03-0.12 μg/kg and 0.1-0.4 μg/kg, respectively.At three different concentration levels, the average recoveries were 77.3%-99.2%, and the relative standard deviations were 0.4%-5.2%.This method offers a simple, green and low-cost alternative for the rapid qualitative and quantitative analysis of 4 kinds of aflatoxins in silkworm pupae powder.

参考文献

[1] 周亚西, 王点点, 段昊, 等.蚕蛹的功能活性及其在保健食品中的应用进展[J].食品安全质量检测学报, 2023, 14(15):241-251.
ZHOU Y X, WANG D D, DUAN H, et al.Functional activity of silkworm pupae and its application progress in health food in China[J].Journal of Food Safety & Quality, 2023, 14(15):241-251.
[2] WU X L, HE K, VELICKOVIC T C, et al.Nutritional, functional, and allergenic properties of silkworm pupae[J].Food Science & Nutrition, 2021, 9(8):4655-4665.
[3] MENTANG F, MAITA M, USHIO H, et al.Efficacy of silkworm (Bombyx mori L.) chrysalis oil as a lipid source in adult Wistar rats[J].Food Chemistry, 2011, 127(3):899-904.
[4] GE S M, TONG X Y, GAO C F, et al.Kinetics of silkworm pupae protein extraction at different ultrasonic frequency and temperature:Effects on physicochemical properties, functional properties and oxidation resistance[J].Process Biochemistry, 2022, 122:36-52.
[5] CAI M, ZHANG Q, GUO P, et al.Comprehensive quality control of silkworm chrysalis using chemical fingerprints combined with antioxidant activity and acetylcholine content[J].Journal of Chromatography A, 2024, 1730:465168.
[6] 王东旭, 陈晓平.高效液相色谱法测定蚕蛹粉中的黄曲霉毒素含量[J].蚕业科学, 2020, 46(1):124-128.
WANG D X, CHEN X P.Determination of aflatoxin content in silkworm Pupa powder by high-performance liquid chromatography[J].Acta Sericologica Sinica, 2020, 46(1):124-128.
[7] LOI M, LOGRIECO A F, PUSZTAHELYI T, et al.Advanced mycotoxin control and decontamination techniques in view of an increased aflatoxin risk in Europe due to climate change[J].Frontiers in Microbiology, 2023, 13:1085891.
[8] KUMAR P, MAHATO D K, KAMLE M, et al.Aflatoxins:A global concern for food safety, human health and their management[J].Frontiers in Microbiology, 2017, 7:2170.
[9] JALLOW A, XIE H L, TANG X Q, et al.Worldwide aflatoxin contamination of agricultural products and foods:From occurrence to control[J].Comprehensive Reviews in Food Science and Food Safety, 2021, 20(3):2332-2381.
[10] International Agency for Research on Cancer.Monographs on the Evaluation of Carcinogenic Risks to Humans[M].Lyon:IARC Press, 1993.
[11] 王蓓蓓, 陈琛, 李崇勇, 等.食品中黄曲霉毒素的前处理与检测方法进展[J].粮食与油脂, 2021, 34(11):1-5.
WANG B B, CHEN C, LI C Y, et al.Advances in pretreatment and detection methods of aflatoxin in food[J].Cereals & Oils, 2021, 34(11):1-5.
[12] 张萍, 彭西甜, 冯钰锜.食品中黄曲霉毒素检测的样品前处理技术研究进展[J].分析科学学报, 2018, 34(2):274-280.
ZHANG P, PENG X T, FENG Y Q.Research advances of sample preparation methods for detection of aflatoxin in food[J].Journal of Analytical Science, 2018, 34(2):274-280.
[13] DU B B, WANG P L, XIAO C, et al.Antibody-free colorimetric determination of total aflatoxins by mercury(II)-mediated aggregation of lysine-functionalized gold nanoparticles[J].Microchimica Acta, 2016, 183(4):1493-1500.
[14] 王东旭, 王新财, 王凤丽, 等.挥发性铵盐盐析辅助液液萃取结合超高效液相色谱-串联质谱法测定酱油中4种黄曲霉毒素[J].食品安全质量检测学报, 2022, 13(14):4634-4640.
WANG D X, WANG X C, WANG F L, et al.Determination of 4 kinds of aflatoxins in soy sauce by volatile salting-out assisted liquid-liquid extraction combined with ultra performance liquid chromatography-tandem mass spectrometry[J].Journal of Food Safety & Quality, 2022, 13(14):4634-4640.
[15] 李丽, 吴宇, 王海波, 等.全自动免疫亲和固相萃取超高效液相色谱法测定粮油中黄曲霉毒素[J].中国粮油学报, 2020, 35(7):157-164.
LI L, WU Y, WANG H B, et al.High throughput method for analysis of aflatoxins in cereals and oils using automated immunoaffinity cleaning up and ultra-high performance liquid chromatography[J].Journal of the Chinese Cereals and Oils Association, 2020, 35(7):157-164.
[16] 郝铖, 王思齐, 李腾飞, 等.分子印迹技术在黄曲霉毒素检测中的最新研究进展[J].分析试验室, 2022, 41(3):350-356.
HAO C, WANG S Q, LI T F, et al.Recent research advances in aflatoxin detection by molecular imprinting technique[J].Chinese Journal of Analysis Laboratory, 2022, 41(3):350-356.
[17] MASSAROLO K C, MENDOZA J R, VERMA T, et al.Fate of aflatoxins in cornmeal during single-screw extrusion:A bioaccessibility approach[J].LWT, 2021, 138:110734.
[18] GUO L, SHAO Y N, DUAN H, et al.Magnetic quantum dot nanobead-based fluorescent immunochromatographic assay for the highly sensitive detection of aflatoxin B1 in dark soy sauce[J].Analytical Chemistry, 2019, 91(7):4727-4734.
[19] LIU Y, LI W, DING Z, et al.Three-dimensional ordered macroporous magnetic photonic crystal microspheres for enrichment and detection of mycotoxins (II):The application in liquid chromatography with fluorescence detector for mycotoxins[J].Journal of Chromatography A, 2019, 1604:460475.
[20] DONG X Q, ZOU B, ZHAO X Y, et al.Rapid qualitative and quantitative analysis of aflatoxin B1 in Pu-erh tea by liquid chromatography-isotope dilution tandem mass spectrometry coupled with the QuEChERS purification method[J].Analytical Methods, 2018, 10(39):4776-4783.
[21] HIDALGO-RUIZ J L, ROMERO-GONZÁLEZ R, MARTÍNEZ VIDAL J L, et al.A rapid method for the determination of mycotoxins in edible vegetable oils by ultra-high performance liquid chromatography-tandem mass spectrometry[J].Food Chemistry, 2019, 288:22-28.
[22] BALLESTEROS-GÓMEZ A, RUBIO S, PÉREZ-BENDITO D.Potential of supramolecular solvents for the extraction of contaminants in liquid foods[J].Journal of Chromatography A, 2009, 1216(3):530-539.
[23] 覃国顺, 吴丹, 龙欣琦, 等.超分子溶剂-微萃取技术在食品及环境污染物检测中的应用进展[J].食品安全质量检测学报, 2025, 16(14):128-138.
QIN G S, WU D, LONG X Q, et al.Progress in the application of supramolecular solvent-microextraction technology in detection of food and environmental pollutants[J].Journal of Food Safety & Quality, 2025, 16(14):128-138.
[24] GARCÍA-FONSECA S, BALLESTEROS-GÓMEZ A, RUBIO S.Restricted access supramolecular solvents for sample treatment in enzyme-linked immuno-sorbent assay of mycotoxins in food[J].Analytica Chimica Acta, 2016, 935:129-135.
[25] 高慧宇, 王国栋, 赵佳, 等.近红外光谱测定小麦粉常规营养成分的模型优化[J].中国食物与营养, 2021, 27(5):30-34.
GAO H Y, WANG G D, ZHAO J, et al.Model optimization for determination of common nutritional components in wheat flour using near infrared spectroscopy[J].Food and Nutrition in China, 2021, 27(5):30-34.
[26] WANG D X, WANG X C, HU Q J, et al.Salting-out assisted liquid-liquid extraction coupled to dispersive liquid-liquid microextraction for the determination of bisphenol A and six analogs (B, E, F, S, BADGE, BFDGE) in canned coffee drinks by ultra-performance liquid chromatography-tandem mass spectrometry[J].Food Analytical Methods, 2021, 14(3):441-452.
[27] BALLESTEROS-GÓMEZ A, RUBIO S.Environment-responsive alkanol-based supramolecular solvents:Characterization and potential as restricted access property and mixed-mode extractants[J].Analytical Chemistry, 2012, 84(1):342-349.
[28] 叶钉利. 超分子溶剂的制备表征及其在中药活性成分提取中的应用[D].长春:长春工业大学, 2024.
YE D L.Preparation, characterization and application of supramolecular solvents in the extraction of active components from traditional Chinese medicine[D].Changchun:Changchun University of Technology, 2024.
[29] SÁNCHEZ-VALLEJO C, BALLESTEROS-GÓMEZ A, RUBIO S.Tailoring composition and nanostructures in supramolecular solvents:Impact on the extraction efficiency of polyphenols from vegetal biomass[J].Separation and Purification Technology, 2022, 292:120991.
文章导航

/

〈 〉