Establishment and evaluation of LC-MS/MS method for ten mycotoxins in Xiangpai brine

  • AI Daoying ,
  • ZHENG Yirou ,
  • HUANG Zhanrui ,
  • ZHAO Liangzhong ,
  • LIN Lidan ,
  • ZHOU Hengping ,
  • ZHOU Kai ,
  • ZHOU Jinsong ,
  • YIN Shixian
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  • 1(College of Food and Chemical Engineering, Shaoyang University, Hunan Provincial Key Laboratory of Soybean Products Processing and Safety Control, Shaoyang 422000, China)
    2(Department of Industry-University-Research Collaboration, Shenzhen Total-Test Technology Co.Ltd., Guangdong Engineering Research Center of High Specificity Biological Rapid Detection, Shenzhen 518038, China)
    3(Pingjiang Jinzai Food Co.Ltd., Yueyang 414000, China)

Received date: 2022-06-22

  Revised date: 2022-07-20

  Online published: 2023-03-03

Abstract

This study established a method for the determination of ten mycotoxins in Xiangpai brine, and carried out methodological validation and actual sample detection based on high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS). The sample (added with isotope internal standard synchronously) was extracted by ultrasound and centrifugation with V(acetonitrile)∶V(water)∶V(acetic acid) =84∶15∶1, and the supernatant was diluted and purified with water. Methanol-water solution was used as mobile phase gradient elution, and electrospray positive and negative multi-reaction ion monitoring mode was adopted. Qualitative and quantitative analysis was carried out by isotope internal standard quantitative method. The results showed that the linearity of the ten mycotoxins were good in the range of 10-200 μg/L (R2>0.998 5), and the limits of detection and quantification were 0.1-13.0 μg/kg and 0.3-40.0 μg/kg, respectively. The spiked recoveries of the ten mycotoxins at the three concentration levels were 78.6%-107.3%, and the relative standard deviations were 2.2%-14.0%, which met the requirements of methodology. The method is easy to operate, and the recovery rate, sensitivity and detection limit all meet the methodological requirements. Thus, this method is suitable for the determination of ten mycotoxins in brine.

Cite this article

AI Daoying , ZHENG Yirou , HUANG Zhanrui , ZHAO Liangzhong , LIN Lidan , ZHOU Hengping , ZHOU Kai , ZHOU Jinsong , YIN Shixian . Establishment and evaluation of LC-MS/MS method for ten mycotoxins in Xiangpai brine[J]. Food and Fermentation Industries, 2023 , 49(3) : 306 -313 . DOI: 10.13995/j.cnki.11-1802/ts.032719

References

[1] 伍涛, 彭希林, 赵良忠, 等.湘派豆干及卤汁在卤制过程中的变化规律[J].食品与发酵工业, 2021, 47(19):146-154.
WU T, PENG X L, ZHAO L Z, et al.Variation law of Xiangpai dried tofu and brine during marinating process[J].Food and Fermentation Industries, 2021, 47(19):146-154.
[2] 陈浩, 杨莹, 赵良忠, 等.湘派卤汁循环使用安全监测及预警模型的构建[J].食品与发酵工业, 2020, 46(21):181-187.
CHEN H, YANG Y, ZHAO L Z, et al.The safety monitoring and early-warning model construction for Xiangpai brine recycling[J].Food and Fermentation Industries, 2020, 46(21):181-187.
[3] 成亚斌, 黄凯信, 宋贤良, 等.不同卤制次数的盐焗鸡卤汁中的营养成分变化规律[J].食品与发酵工业, 2014, 40(3):129-133.
CHENG Y B, HUANG K X, SONG X L, et al.The nutrition change in the brine of water-boiled salted chicken with different marinating times[J].Food and Fermentation Industries, 2014, 40(3):129-133.
[4] LIU Y, XU X L, ZHOU G H.Changes in taste compounds of duck during processing[J].Food Chemistry, 2007, 102(1):22-26.
[5] 刘登勇, 刘欢, 张庆永, 等.反复卤煮过程中扒鸡卤汤物理及感官特性变化分析[J].食品科学, 2017, 38(11):116-121.
LIU D Y, LIU H, ZHANG Q Y, et al.Changes in physical and sensory characteristics of Dezhou braised chicken brine during repeated braising[J].Food Science, 2017, 38(11):116-121.
[6] 邵俊锋, 李波, 陆炀, 等.基于主成分分析法的盐水鹅老卤风味强度评价模型的构建[J].食品与发酵工业, 2020, 46(14):262-268.
SHAO J F, LI B, LU Y, et al.Construction of evaluation model for flavor intensity of salted goose aged brine based on principal component analysis[J].Food and Fermentation Industries, 2020, 46(14):262-268.
[7] 肖凌云.武冈卤制品产业发展现状及HACCP体系应用研究[D].长沙:湖南农业大学, 2015.
XIAO L Y.The development status of thick gravy-food in Wugang and the application of HACCP system[D].Changsha:Hunan Agricultural University, 2015.
[8] 杜垒, 谢伟, 徐幸莲, 等.复卤前后盐水鸭老卤基本成分与安全指标变化[J].食品科学, 2009, 30(13):101-104.
DU L, XIE W, XU X L, et al.Changes of main components of old brine used in production of water-boiled salted duck and determination of safety indexes before and after rebrining[J].Food Science, 2009, 30(13):101-104.
[9] 吴俊师, 刘巧瑜, 陈俊文, 等.重复卤制对卤汁品质的影响[J].中国调味品, 2021, 46(7):70-75.
WU J S, LIU Q Y, CHEN J W, et al.Effect of repeated marinating on the quality of marinade[J].China Condiment, 2021, 46(7):70-75.
[10] 何卓霖, 李子琨, 穆蕾, 等.同位素内标-高效液相色谱-串联质谱法同时测定小麦和玉米中19种真菌毒素[J].中国粮油学报, 2022, 37(7):150-157.
HE Z L, LI Z K, MU L, et al.Simultaneous determination of isotope internal standard-high performance liquid chromatography-tandem mass spectrometry 19 mycotoxins in wheat and corn[J].Journal of the Chinese Cereals and Oils Association, 2022, 37(7):150-157.
[11] DEMISSIE N.A review of aflatoxin:Occurrence, prevention, and gaps in both food and feed safety[J].Novel Techniques in Nutrition & Food Science, 2018, 1(3):35-43.
[12] YANG C, SONG G, LIM W.Effects of mycotoxin-contaminated feed on farm animals[J].Journal of Hazardous Materials, 2020, 389:122087.
[13] 杨帅, 杨永坛, 穆蕾, 等.液相色谱-串联质谱同时测定食用植物油中的多种真菌毒素[J].中国食品学报, 2021, 21(5):309-316.
YANG S, YANG Y T, MU L, et al.Simultaneous detection of multi-mycotoxins in edible oil using liquid chromatography tandem mass spectrometry[J].Journal of Chinese Institute of Food Science and Technology, 2021, 21(5):309-316.
[14] 胡佳哲, 赖宇红, 陈浩桉.中药材中常见真菌毒素污染状况及分析方法研究进展[J].海峡药学, 2019, 31(1):1-5.
HU J Z, LAI Y H, CHEN H A.Research progress of the pollution status and analysis methods of common fungal toxins in Chinese medicinal herbs[J].Strait Pharmaceutical Journal, 2019, 31(1):1-5.
[15] 韦芳, 廖晓芳, 刘晓菲, 等.中药材等复杂基质中真菌毒素检测的前处理技术研究新进展[J].中国中药杂志, 2018, 43(17):3 431-3 443.
WEI F, LIAO X F, LIU X F, et al.Research progress of pretreatment technology for mycotoxin detection in Chinese materia medica and complex matrices[J].China Journal of Chinese Materia Medica, 2018, 43(17):3 431-3 443.
[16] 管卓龙, 卢跃鹏, 侯靖, 等.高效液相色谱-串联质谱法同时测定蒸肉粉中6种真菌毒素[J].食品科技, 2021, 46(5):295-300.
GUAN Z L, LU Y P, HOU J, et al.Determination of 6 mycotoxin contaminants in rice flour for steamed pork by high performance liquid chromatography-tandem mass spectrometry[J].Food Science and Technology, 2021, 46(5):295-300.
[17] 刘新, 张凤兵, 王鸿, 等.基于主成分分析和聚类分析的老卤汁产品品质评价[J].食品科技, 2020, 45(3):274-278.
LIU X, ZHANG F B, WANG H, et al.Evaluation of marinades quality based on principal component analysis and hierarchical cluster analysis[J].Food Science and Technology, 2020, 45(3):274-278.
[18] 吴红涛, 李萌萌, 关二旗, 等.四极杆-轨道阱液质联用法同时检测玉米中四种真菌毒素[J].食品与发酵工业, 2022,48(24):245-251.
WU H T, LI M M, GUAN E Q, et al.Simultaneous determination of four mycotoxins in maize by Quadrupole-Orbitrap LC-MS[J].Food and Fermentation Industries, 2022,48(24):245-251.
[19] 徐洪文, 朱瑜, 徐华, 等.高效液相色谱法测定食用植物油中6种真菌毒素[J].中国油脂, 2020, 45(11):77-83.
XU H W, ZHU Y, XU H, et al.Detection of six mycotoxins in edible vegetable oil by high performance liquid chromatography[J].China Oils and Fats, 2020, 45(11):77-83.
[20] WALL-MARTÍNEZ H A, PASCARI X, RAMOS A J, et al.Frequency and levels of mycotoxins in beer from the Mexican market and exposure estimate for deoxynivalenol mycotoxins[J].Mycotoxin Research, 2019, 35(2):207-216.
[21] GONZÁLEZ-JARTÍN J M, ALFONSO A, RODRÍGUEZ I, et al.A QuEChERS based extraction procedure coupled to UPLC-MS/MS detection for mycotoxins analysis in beer[J].Food Chemistry, 2019, 275:703-710.
[22] 王权帅, 孙卫明.同位素内标-超高效液相色谱-串联质谱法同时测定板栗中16种真菌毒素[J].食品科技, 2021, 46(11):307-313.
WANG Q S, SUN W M.Simultaneous determination of 16 kinds of mycotoxins in chestnut using isotope internal standard-high performance liquid chromatography–tandem mass spectrometry[J].Food Science and Technology, 2021, 46(11):307-313.
[23] 苏萌, 艾连峰.液相色谱-串联质谱基质效应及其消除方法[J].食品安全质量检测学报, 2014(2):511-515.
SU M, AI L F.Matrix effects and elimination methods of liquid chromatography-tandem mass spectrometry[J].Journal of Food Safety & Quality, 2014(2):511-515.
[24] FRENICH A G, ROMERO-GONZÁLEZ R, GÓMEZ-PÉREZ M L, et al.Multi-mycotoxin analysis in eggs using a QuEChERS-based extraction procedure and ultra-high-pressure liquid chromatography coupled to triple quadrupole mass spectrometry[J].Journal of Chromatography A, 2011, 1218(28):4 349-4 356.
[25] 孙嘉笛, 徐洪文, 徐一达, 等.食用植物油中黄曲霉毒素和赭曲霉毒素的污染状况及特征分析[J].中国油脂, 2022, 47(9):35-43.
SUN J D, XU H W, XU Y D, et al.Analysis of contamination status and characteristics of aflatoxin and ochratoxin in edible vegetable oils[J].China Oils and Fats, 2022, 47(9):35-43.
[26] 吴宇, 叶金, 张冰, 等.稳定同位素稀释-超高效液相色谱-串联质谱法快速测定植物油中16种真菌毒素[J].分析化学, 2018, 46(6):975-984.
WU Y, YE J, ZHANG B, et al.A fast analytical approach for determination of 16 kinds of mycotoxins in vegetable oils using stable isotope dilution and ultra high performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry, 2018, 46(6):975-984.
[27] 李峻媛, 万丽, 杨美华.真菌毒素限量标准及其在中药中的研究进展[J].中草药, 2011, 42(3):602-609.
LI J Y, WAN L, YANG M H.Limit standard of mycotoxins and advances in studies on its application in Chinese materia medica[J].Chinese Traditional and Herbal Drugs, 2011, 42(3):602-609.
[28] YANG M H, CHEN J M, ZHANG X H.Immunoaffinity column clean-up and liquid chromatography with post-column derivatization for analysis of aflatoxins in traditional Chinese medicine[J].Chromatographia, 2005, 62(9-10):499-504.
[29] ROMAGNOLI B, MENNA V, GRUPPIONI N, et al.Aflatoxins in spices, aromatic herbs, herb-teas and medicinal plants marketed in Italy[J].Food Control, 2007, 18(6):697-701.
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