高效液相色谱-串联质谱法测定果汁中恩镰孢菌素和白僵菌素
PDF下载 (251)邓 涛,吉小凤,肖英平,汪 雯,吕文涛,王小骊,吴 振,杨 华.高效液相色谱-串联质谱法测定果汁中恩镰孢菌素和白僵菌素[J].宁波大学学报(理工版),2023,36(6):50-56.DOI:10.20098/j.cnki.1001-5132.2022.1006
DENG Tao,JI Xiaofeng,XIAO Yingping,WANG Wen,L? Wentao,WANG Xiaoli,WU Zhen,YANG Hua.Determination of enniatins and beauvericin in fruit juice by high performance liquid chromatography-tandem mass spectrometry[J].Journal of Ningbo University(Natural Science & Engineering Edition),2023,36(6):50-56.DOI:10.20098/j.cnki.1001-5132.2022.1006
| Title: | Determination of enniatins and beauvericin in fruit juice by high performance liquid chromatography-tandem mass spectrometry |
| 作者: | 邓 涛, 吉小凤, 肖英平, 汪 雯, 吕文涛, 王小骊, 吴 振, 杨 华 |
| Author(s): | DENG Tao, JI Xiaofeng, XIAO Yingping, WANG Wen, L? Wentao, WANG Xiaoli, WU Zhen, YANG Hua |
| 关键词: | 果汁; 恩镰孢菌素; 白僵菌素; 食品安全 |
| Keywords: | fruit juice; enniatins; beauvericin; food safety |
| 分类号: | O675.63; TS201.6 |
| DOI: | 10.20098/j.cnki.1001-5132.2022.1006 |
| 文献标识码: | A |
| 摘要: | 建立高效液相色谱-串联质谱法测定果汁中恩镰孢菌素和白僵菌素检测方法. 样品用V(乙腈)V(水)V(甲酸)混合液(79201)提取, QuEChERS填料包(无水MgSO4、0无水CH3COONa和 NaCl)盐析, 100mg C18净化, 经过液相色谱柱分离, 2mmol·L–1乙酸铵水溶液-甲醇为流动相梯度洗脱, 由ESI源扫描, 多反应监测模式, 基质外标法定量分析. 该方法中, 恩镰孢菌素A(ENA)、恩镰孢菌素B(ENB)和白僵菌素(BEA)在0.1~200μg·L–1以及恩镰孢菌素A1(ENA1)和恩镰孢菌素B1(ENB1)在1~200μg·L–1范围内线性关系良好, 且线性相关系数(R2)均大于0.9989, 相对标准偏差范围为1.7%~11.7%. 3个不同加标浓度的添加回收率为88.0%~114.1%, 样品检测限为1.5?g·kg–1, 样品定量限为5?g·kg–1. 本文建立的方法简单、高效、准确, 满足果汁中恩镰孢菌素和白僵菌素污染筛查需求. |
| Abstract: | A high performance liquid chromatography-tandem mass spectrometry method was developed for the simultaneous determination of enniatins and beauvericin in fruit juices. Samples were extracted with V(acetonitrile)V(water)V(formic acid) mixture solution (79201), salted out extraction by QuEChERS packed packages ( anhydrous MgSO4, anhydrous CH3COONa and NaCl), purified by 100mg C18, and separated by liquid chromatography column with 2mmol·L–1 ammonium acetate aqueous solution-methanol as mobile phase gradient elution. ESI positive ion mode scanning, multiple response monitoring mode detection, and matrix external standard method quantitative analysis were employed. The linearity was in the range of 0.1-200μg·L–1 for ENA、ENB and BEA, and the linearity was in the range of 1-200μg·L–1 for ENA1 and ENB1, with the correlation coefficients (R2) greater than 0.9989 and relative standard deviations ranging from 1.7% to 11.7%. The recoveries were ranged from 88.0% to 114.1%. The samples’ limits of detection were 1.5μg·kg–1, and their limits of quantitation were 5μg·kg–1. The method established in this study is demonstrated as being simple, efficient, and accurate, which can satisfy the requirements of screening tests for enniatins and beauvericin in fruit juice samples. |
| 参考文献 /References: | [1] 史文景. 柑橘和果汁中链格孢霉毒素检测技术研究[D]. 重庆: 西南大学, 2014. [2] Yang Y, Li G L, Wu D, et al. Recent advances on toxicity and determination methods of mycotoxins in foodstuffs [J]. Trends in Food Science & Technology, 2020, 96: 233-252. [3] 王玉娇. 坚果和干果真菌毒素污染及风险评估研究[D]. 北京: 中国农业科学院, 2018. [4] Maranghi F, Tassinari R, Narciso L, et al. In vivo toxicity and genotoxicity of beauvericin and enniatins: Combined approach to study in vivo toxicity and genotoxicity of mycotoxins beauvericin (BEA) and enniatin B (ENNB)[J]. EFSA Supporting Publications, 2018, 15(5):1-18. [5] Stanciu O, Juan C, Miere D, et al. Analysis of enniatins and beauvericin by LC-MS/MS in wheat-based products [J]. Journal of Food, 2017, 15(3):433-440. [6] 秦露, 张磊, 蒋佳伊, 等. 基于酶联免疫分析法高通量筛查中药材中赭曲霉毒素A的污染研究[J]. 中国中药杂志, 2019, 44(23):5072-5077. [7] Beyene A M, Du X W, Schrunk E D, et al. High-performance liquid chromatography and enzyme- linked immunosorbent assay techniques for detection and quantification of aflatoxin B feed samples: A comparative study[J]. BMC Research Notes, 2019, 12(1):492. [8] Rizzo I, Vedoya G, Maurutto S, et al. Assessment of toxigenic fungi on Argentinean medicinal herbs[J]. Microbiological Research, 2004, 159(2):113-120. [9] 谭洪波. 粮油中真菌毒素检测技术及其应用解析[J]. 现代食品, 2019(21):166-168. [10] Font G, Rodríguez-Carrasco Y, Moltó J C, et al. Monitoring Alternaria mycotoxins and pesticide residues in tomato by dispersive liquid-liquid microextraction coupled to gas chromatography-tandem mass spectro- metry[J]. Toxicology Letters, 2013, 221:S122. [11] 李春扬, 张晓磊, 田菲菲, 等. 气相色谱-串联质谱技术在食品分析中的应用研究进展[J]. 食品安全质量检测学报, 2016, 7(8):3291-3299. [12] Dias J V, da Siva R C, Pizzutti I R, et al. Patulin in apple and apple juice: Method development, validation by liquid chromatography-tandem mass spectrometry and survey in Brazilian south supermarkets[J]. Journal of Food Composition and Analysis, 2019, 82:103242. [13] 王远, 邢丽杰, 李先义, 等. UPLC-MS/MS法测定番茄酱中5种链格孢霉毒素[J]. 食品工业, 2021, 42(7):323- 327. [14] Prelle A, Spadaro D, Garibaldi A, et al. A new method for detection of five alternaria toxins in food matrices based on LC-APCI-MS[J]. Food Chemistry, 2013, 140(1/2): 161-167. [15] Wang M, Jiang N, Xian H, et al. A single-step solid phase extraction for the simultaneous determination of 8 mycotoxins in fruits by ultra-high performance liquid chromatography tandem mass spectrometry[J]. Journal of Chromatography A, 2016, 1429:22-29. [16] 李磊, 韦柳丹, 周贻兵, 等. 固相萃取净化-超高效液相色谱串联质谱法测定菜籽油中交链孢霉毒素含量[J]. 中国油脂, 2021, 46(8):119-122; 139. [17] 阳曦, 刘玮, 向世杰. 液液萃取-全碳同位素标记-液质联用法测定酱油中玉米赤霉烯酮[J]. 中国调味品, 2021, 46(11):151-154. [18] 蒋林惠, 陈彬, 周易枚, 等. QuEChERS-液质联用技术同时测定大米中的4种真菌毒素及5种农药残留量方法的研究[J]. 粮食与食品工业, 2021, 28(5):54-58. [19] Jo H W, Park M K, Heo H M, et al. Simultaneous determination of 13 mycotoxins in feedstuffs using QuEChERS extraction[J]. Applied Biological Chemistry, 2021, 64(1):1-12. [20] 赵英莲, 张梓琪, 赵鑫, 等. QuEChERS技术在食品真菌毒素检测中的研究进展[J]. 中国酿造, 2020, 39(1): 1-5. [21] 方真, 曲栗, 古淑青, 等. 加速溶剂萃取-QuEChERS-超高效液相色谱-串联质谱法测定药食同源性食品中16种真菌毒素[J]. 色谱, 2020, 38(7):782-790. [22] 许娇娇, 黄百芬, 周健, 等. 直接稀释-超高效液相色谱-串联质谱法快速测定谷物及其制品中16种真菌毒素[J]. 中国食品卫生杂志, 2017, 29(6):708-715. [23] Ji X F, Li R, Yang H, et al. Occurrence of patulin in various fruit products and dietary exposure assessment for consumers in [J]. Food Control, 2017, 78:100- 107. [24] Li X J, Li H M, Li X M, et al. Determination of trace patulin in apple-based food matrices[J]. Food Chemistry, 2017, 233:290-301. [25] Trufelli H, Palma P, Famiglini G, et al. An overview of matrix effects in liquid chromatography-mass spectrometry [J]. Mass Spectrometry Reviews, 2011, 30(3):491-509. |
| 备注/Memo: | 收稿日期:2022-10-12.宁波大学学报(理工版)网址:http://journallg.nbu.edu.cn/ 基金项目:科技部国家重点研发计划政府间合作项目(2019YFE0103900). 第一作者:邓涛(1997-),男,安徽滁州人,在读硕士研究生,主要研究方向:食品安全与营养.E-mail:dengtao8822@163.com *通信作者:吴振(1985-),男,河南新乡人,博士/副教授,主要研究方向:食品加工与安全.E-mail:wuzhen@nbu.edu.cn 宁波大学学报(理工版)网址:http://journallg.nbu.edu.cn/ |